反应详情

Reflux a stirred mixture of dimethyl-thiocarbamic acid S-(4-acetyl-3-hydroxy-2-propyl-phenyl)ester (1.08 g, 3.84 mmol), potassium hydroxide (1.1 g, 19.2 mmol), ethanol (25 mL), and water (10 mL) for 2 hours. Cool the reaction in an ice/water bath and adjust the pH to 2 with aqueous 5N hydrochloric acid. Extract the mixture with ethyl acetate (3×50 mL). Combine the extracts and wash with water (50 mL) and brine (50 mL) and dry over magnesium sulfate, filter, and concentrate to afford the title compound (0.76 g, 94%) as a brown oil which solidifies on standing. LCMS (m/z) 211 M−1.

1. temperatureReflux
2. temperatureCool
3. customthe reaction in an ice/water bath
4. extractionExtract the mixture with ethyl acetate (3×50 mL)
5. washCombine the extracts and wash with water (50 mL) and brine (50 mL)
6. dry with materialdry over magnesium sulfate
7. filtrationfilter
8. concentrationconcentrate