2-(3-Fluorophenyl)-3-methylmorpholine (3-Fluorophenmetrazine)

Page 1

Reaxys

PubChem

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Reactions (3)

Substances (3)

Citations (3)

Structure

Structure/Compound Data Chemical Name: 2-(3-fluoro-phenyl)-3-methyl-morpholine Reaxys Registry Number: 22041177

CAS Registry Number: 1350768-28-3 Molecular Formula: C11H14FNO Linear Structure Formula: C11H14FNO Molecular Weight: 195.237 InChI Key: VHYVKJAQSJCYCK-UHFFFAOYSA-N

N° of preparations All Preps | All Reactions 1 prep out of 2 reactions.

Available Data

N° of ref.

Identification Bioactivity (8)

3

1

Synthesize | Hide Details Find similar Chemical Names and Synonyms 2-(3-fluoro-phenyl)-3-methyl-morpholine, 2-(3-fluorophenyl)-3-methylmorpholine, PAL-593 Identification Patent-Specific Data (1) Related Markush Structure (RN) 22041163; 22041164

Reference RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

Bioactivity


Pharmacological Data (8) 1 of 8

Comment (Pharmacological Data)

Bioactivities present

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

Bäckberg, Matilda; Westerbergh, Jenny; Beck, Olof; Helander, Anders

Clinical Toxicology, 2016 , vol. 54, # 9 p. 819 - 825 Title/Abstract Full Text View citing articles Show Details

McLaughlin, Gavin; Morris, Noreen; Kavanagh, Pierce V.; Dowling, Geraldine; Power, John D.; Twamley, Brendan; O'Brien, John; Talbot, Brian; Sitte, Harald H.; Brandt, Simon D.

Drug Testing and Analysis, 2017 , vol. 9, # 3 p. 369 - 377 Title/Abstract Full Text Show Details

2 of 8

Effect (Pharmacological Data)

dopamine (DA); release of

Species or TestSystem (Pharmacological Data)

caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test.

Results

release (percent) = 100 at 10 μmol/l

Location

Page/Page column 81-82; 84

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

3 of 8

Effect (Pharmacological Data)

serotonin (5-HT); release of

Species or TestSystem (Pharmacological Data)

whole brain minus cerebellum and caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal


preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test. Results

release (percent) = 95 at 10 μmol/l

Location

Page/Page column 81-82; 84

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

4 of 8

Effect (Pharmacological Data)

norepinephrine (NE); release of

Species or TestSystem (Pharmacological Data)

whole brain minus cerebellum and caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test.

Results

release (percent) = 93 at 10 μmol/l

Location

Page/Page column 81-82; 84

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

5 of 8

Effect (Pharmacological Data)

serotonin (5-HT2B) receptor; antagonist

Species or TestSystem (Pharmacological Data)

whole brain minus cerebellum and caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to


block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test. Results

antagonist (percent) = 1 at 10 μmol/l

Location

Page/Page column 81-82; 84

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

6 of 8

Effect (Pharmacological Data)

dopamine (DA); release of

Species or TestSystem (Pharmacological Data)

caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test.

Type (Pharmacological Data)

EC50

Value of Type (Pharmacological Data)

43 nmol/l

Location

Page/Page column 81-82; 85

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

7 of 8

Effect (Pharmacological Data)

serotonin (5-HT); release of


Species or TestSystem (Pharmacological Data)

whole brain minus cerebellum and caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test.

Type (Pharmacological Data)

EC50

Value of Type (Pharmacological Data)

2558 nmol/l

Location

Page/Page column 81-82; 85

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

8 of 8

Effect (Pharmacological Data)

norepinephrine (NE); release of

Species or TestSystem (Pharmacological Data)

whole brain minus cerebellum and caudate of rat

Method (Pharmacological Data)

Example 4 - DA, NE, 5-HT Release AssaysA series of compounds were assayed for release of dopamine, serotonin, and norepinephrine as well as for activity at the 5-HT2B receptor. This data is shown below in Table 3.DA, NE and 5-HT Release Assays[3H]MPP+ was used as the

radioligand for both the DA and NE release assays, because this method led to an improved signal-to-noise ratio. Rat caudate (for DA release) or whole brain minus cerebellum and caudate (for NE and 5-HT release), was homogenized in ice-cold 10percent sucrose containing 1 μΜ reserpine. Nomifensine (100 nM) and GBR12935 (100 nM) were added to the sucrose solution for [3H]5-HT release experiments to block any potential [3H]5-HT reuptake into NE and DA nerve terminals. For the DA release assay, 100 nM desipramine and 100 nM citalopram were added to block [3H]MPP+ uptake into NE and 5-HT nerves. For the NE release assay, 50 nMGBR12935 and 100 nM citalopram were added to block [3H]MPP+ uptake into DA and 5-HT nerves. After 12 strokes with a Potter-Elvehjem homogenizer, homogenates were centrifuged at 1000 x g for 10 min at 0^1 °C and the supernatants were retained on ice (synaptosomal preparation).Synaptosomal preparations were incubated to steady state with 5 nM [3H]MPP+ (60 min) or 5 nM [3H]5-HT (60 min) in Krebsphosphate buffer (without BSA) (pH 7.4), which contained 154.4 mM aCl, 2.9 mM KC1, 1.1 mM CaCl2, 0.83 mM MgCl2, 5 mM glucose, 1 mg/mL ascorbic acid, 50 μΜ pargyline plus 1 μΜ reserpine in a polypropylene beaker with stirring at 25 °C with the appropriate blockers. After incubation to steady state, 850 μ of synaptosomes preloaded with [3H]ligand were added to 12 x 75 mm polystyrene test tubes that contained 150 μ test drug in uptake buffer plus 1 mg/ml BSA. After 5 min (3H]5-HT) or 30 min (NE and DA assays) the release reaction was terminated by dilution with 4 ml wash buffer (10 mM Tris-HCl pH 7.4 containing 0.9percent NaCl at 25 °C) followed by rapid vacuum filtration over Whatman GF/B filters using a Brandel Harvester. The filters were rinsed twice with 4 ml wash buffer using the Brandel Harvester, and the retained tritium was counted by a Taurus liquid scintillation counter at 40percent efficiency after an overnight extraction in 3 ml Cytoscint (ICN).Substrate Reversal ExperimentsFor substrate reversal experiments, test drugs were tested at approximately EDgo doses in the absence and presence of blockers (250 nM GBR1209 for DAT, 166 nM desipramine for NET, 100 nM fluoxetine for SERT). Substrate activity was detected by a significant reversal of the releasing effect of the test drug.Data analysis and statisticsAs previously described (Rothman RB, Baumann MH, Dersch CM, Romero DV, Rice KC, Carroll FI and Partilla JS Synapse 39: 32-41 (2001), incorporated herein by reference), EC50 values were determined using the nonlinear least squares curve fitting program MLAB-PC (Civilized Software, Bethesda, MD). In substrate reversal experiments, statistical significance was determined using the Student's t-test.

Type (Pharmacological Data)

EC50

Value of Type

30 nmol/l


(Pharmacological Data) Location

Page/Page column 81-82; 85

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

Reaxys Registry Number: 22041319

Molecular Formula: C4H4O4*2C11H14FNO Linear Structure Formula: C4H4O4*2C11H14FNO Molecular Weight: 506.547 InChI Key: JDKZDYTXIAFLLT-WLHGVMLRSA-N

2

2 prep out of 2 reactions.

Identification Spectra (1)

1

Synthesize | Hide Details Find similar

Identification Patent-Specific Data (1) Related Markush Structure (RN)

Reference

22041163; 22041164

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

Spectra NMR Spectroscopy (1) Nucleus (NMR Spectroscopy)

Solvents (NMR Spectroscopy)

Frequency (NMR Spectroscopy)

1H

methanol-d4

300 MHz

Original Text (NMR Spectroscopy)

Location

1H NMR (300 MHz, METHANOL-^) δ ppm 0.96 (d, J-6.78 Hz, 3 H) 3.04 - 3.17 (m, 1 H) 3.17 - 3.24 (m, 1 H) 3.26 (m, 1 H) 3.83 (t, J=l l . l l Hz, 1 H) 4.09 (d, J=1 1.68 Hz, 1 H) 4.23 (d, J=9.42 Hz, 1 H) 6.68 (s, 1 H) 7.03 - 7.24 (m, 3 H) 7.39 (dd, J=7.91, 7.16 Hz, 1 H).

Page/Page column 55

Comment (NMR Spectroscopy) Signals given

Reference RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details

Reaxys Registry Number: 26312870

Molecular Formula: C11H14FNO Linear Structure Formula: C11H14FNO Molecular Weight: 195.237 InChI Key: VHYVKJAQSJCYCK-GZMMTYOYSA-N

3

no reactions.

Bioactivity (1)

1


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Bioactivity Pharmacological Data (1) 1 of 1

Comment (Pharmacological Data)

Bioactivities present

Reference

RESEARCH TRIANGLE INSTITUTE; UNITED STATES OF AMERICA, as represented by THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES, C/O NATIONAL INSTITUTES OF HEALTH, OFFICE OF TECHNOLOGY TRANSFER; BLOUGH, Bruce E.; ROTHMAN, Richard; LANDAVAZO, Antonio; PAGE, Kevin M.; DECKER, Ann Marie

Patent: WO2011/146850 A1, 2011 ; Title/Abstract Full Text Show Details


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