反应详情

温度

0 °C

A solution of 5 g (17.35 mol) of N-[4-cyano-3-trifluoromethyl-phenyl]-2,3-dihydroxy-2-methyl-propionamide in 50 ml of dry pyridine was cooled to 0° C. and 10 g (52.45 mmol) of p-toluenesulfonyl chloride was added in small portions. The mixture was stirred at 0° C. for 5 h, then diluted with 200 ml of dichloromethane, washed three times with 50 ml of saturated aqueous sodium hydrogen carbonate, twice with 50 ml of 10% aqueous hydrochloric acid and 50 ml of brine. The organic layer was dried over sodium sulfate and concentrated in vacuum. The residue was crystallized from a 1:5 mixture of ethyl acetate/petroleum ether, which has a boiling range of 40–70° C.

1. washwashed three times with 50 ml of saturated aqueous sodium hydrogen carbonate
2. dry with materialThe organic layer was dried over sodium sulfate
3. concentrationconcentrated in vacuum
4. customThe residue was crystallized from a 1:5 mixture of ethyl acetate/petroleum ether, which