Method for preparing pure enantio-methylpropane-2-sulfinamide
A technology of tert-butyl sulfinamide and tert-butyl sulfinyl, which is applied in the field of pharmaceutical synthesis, can solve the problems of high cost, unfavorable large-scale production, long overall steps, etc., and achieves reduction of reaction time, convenience for industrial scale-up production, Simple to use effects
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[0042] The first step: the synthesis of tert-butyl thiosulfinate.
[0043] (1) Add 180g of tert-butyl disulfide, 1.8g of VO(acac)2 and 400mL of ethanol to the reaction flask successively, add 138.5g of 27% hydrogen peroxide dropwise at 25°C, react at 30-35°C for 7 hours, sample TLC or HPLC detected that the raw material was less than 1.5%, concentrated under reduced pressure, washed once with saturated sodium chloride water, and then added 400 g of dichloromethane to dilute the sodium sulfate and dry it for later use. The external standard yield was 88%.
[0044] (2) Add 180g tert-butyl disulfide and 420mL acetic acid to the reaction flask successively, add 150.1g 27% hydrogen peroxide dropwise at 25°C, react at 30-35°C for 3 hours, sample TLC or HPLC for detection, the raw material is less than 1% , Then poured into 500g water, extracted with dichloromethane, washed once with saturated sodium chloride water, dried over sodium sulfate for later use. The external standard yield wa...
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