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in ethyl acetate
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Eisai Co., Ltd.
Patent: US5110956 A1, 1992 ; Title/Abstract Full Text Show Details
P.3:2-(1,3-Benzodioxol-5-yl)-1-methylethanethiol STR299 Preparative Example 3 2-(1,3-Benzodioxol-5-yl)-1-methylethanethiol STR299 5 g of anhydrous tin chloride was added to 100 g of safrole. Hydrochloric acid gas was passed though the mixture under cooling with ice for 1.5 hours. 2 l of ethyl acetate was added to the reaction mixture, followed by the dissolution. The obtained mixture was washed with water twice, dried over anhydrous sodium sulfate and distilled to remove the solvent. The residue was purified by silica gel column chromatography (hexane/benzene=10:1) to obtain 41.7 g of 5-(2-chloropropyl)-1,3-benzodioxole as a colorless oil.