反应详情

A solution of the product from Step B, 25 g, in anhydrous dimethylformamide (DMF) (300 ml) was cooled to 0° and 99% NaH, 3.46 g, was added in two portions. The mixture was stirred for 1 hour at 0° then dimethylthiocarbamoyl chloride, 19.3 g, was added and the mixture heated at 90° under a N2 atmosphere for 1.5 hours. The mixture was cooled to room temperature and diluted with water to 1,200 mL. The resulting solution was then extracted with ethyl acetate (3×50 ml). The combined organic layers were washed with brine and then dried over Na2SO4 and evaporated to dryness in vacuo to yield a residue which was purified by chromatography on silica gel to Yield the title compound, mp 62°-64°.

1. temperaturethe mixture heated at 90° under a N2 atmosphere for 1.5 hours
2. extractionThe resulting solution was then extracted with ethyl acetate (3×50 ml)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. customevaporated to dryness in vacuo
6. customto yield a residue which
7. customwas purified by chromatography on silica gel