反应详情

To a solution of methyl 4-(methylthio)-3-(trifluoromethyl)benzoate (10.0 g, 40.0 mmol) in tetrahydrofuran (100 mL) was added lithium aluminum hydride (1.52 g, 40.0 mmol) at 0° C. by small portions, and the resulting mixture was stirred for 15 min. Sodium sulfate decahydrate (12.9 g, 40.0 mmol) was added to the reaction mixture by small portions, and the obtained mixture was further stirred at room temperature for 1 hr. Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=1/1), and crystallized from hexane/ethyl acetate to give the title compound (8.46 g, yield 95%) as colorless crystals.

1. stirringthe obtained mixture was further stirred at room temperature for 1 hr
2. filtrationInsoluble material was filtered off
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=1/1)
5. customcrystallized from hexane/ethyl acetate