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2016-06-04 10h:09m:35s (EST)
O NH 2
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O
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2016-06-04 10:23:42
O
HCl
H 2N O
Rx-ID: 25356466 View in Reaxys 1/1 Yield 75%
Conditions & References R.7 : 2,5-Dimethoxy-3,4-dimethylbenzeneethaneamine hydrochloride Reference Example 7 2,5-Dimethoxy-3,4-dimethylbenzeneethaneamine hydrochloride To a solution of 2,5-dimethoxy-3,4-dimethylbenzeneacetonitrile (20.6 g, 0.100 mol) inethanol (100 mL) were added a saturated ammonia-ethanol solution (250 mL) and Raney nickel (15 g), and the mixture was stirred at 50°C for 2.5 hours under the hydrogen atmosphere (5.5 atmospheres). The catalyst was filtered, and the filtrate was concentrated under reduced pressure. The residue was dissolved in methanol, a 10percent hydrogen chloride-methanol solution (50 mL) was added, and concentrated under the reduced pressure. The residue was recrystallized from methanol-diethyl ether to obtain 18.4 g of the title compound. Yield 75percent mp. 237-240°C 1H-NMR (DMSO-d ) δ 2.04 (3H, s), 2.13 (3H, s), 2.8-3.1 (4H, m), 3.60 (3H, s), 3.75 (3H, s), 6.69 (1H, s), 8.15 (3H, 6 br) Patent; Takeda Chemical Industries, Ltd.; EP1213290; (2002); (A1) English View in Reaxys
Copyright © 2016 Reed Elsevier Properties SA. All rights reserved. Authorized use only. Reaxys® and the Reaxys® trademark are owned and protected by Reed Elsevier Properties SA and used under license.
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2016-06-04 10:23:42