Method of synthesizing enantiomerically pure tert-butanesulfinamide
A technology of tert-butyl sulfinamide and tert-butyl sulfinyl, applied in the field of pharmaceutical synthesis, can solve the problems of high cost, long overall steps, unfavorable large-scale production, etc., and achieves reduced reaction time, simple operation, and convenient industrialization. Amplify the effect of production
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[0042] The first step: the synthesis of tert-butyl thiosulfinate.
[0043] (1) Add 180g tert-butyl disulfide, 1.8gVO(acac)2 and 400mL ethanol successively in the reaction bottle, add 138.5g 27% hydrogen peroxide dropwise at 25°C, react at 30-35°C for 7 hours, take a sample for TLC or According to HPLC detection, the raw material is less than 1.5%, concentrated under reduced pressure, washed once with saturated sodium chloride water, then added 400 g of dichloromethane to dilute sodium sulfate and dried for later use. The external standard yield was 88%.
[0044] (2) Add 180g of tert-butyl disulfide and 420mL of acetic acid in turn to the reaction bottle, add 150.1g of 27% hydrogen peroxide dropwise at 25°C, react at 30-35°C for 3 hours, take a sample for TLC or HPLC detection, and the raw material is less than 1% , then poured into 500g of water, extracted with dichloromethane, washed once with saturated sodium chloride water, dried over sodium sulfate for use. The external ...
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