反应详情

To a solution of 2-chloro-3-oxobutyric acid methyl ester (3.5 g) and 4-chlorobenzenethiol (4.1 g) in dichloromethane (60 mL) at 0° C. was added triethylamine (4.0 mL). The mixture was warmed to room temperature and then stirred at this temperature for 3 days. The solvent was removed under reduced pressure and the residue diluted with ethyl acetate and this mixture was washed with saturated aqueous sodium chloride solution and then dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel, eluting with a mixture of ethyl acetate and cyclohexane (1:4 by volume) to afford title compound as a waxy solid, 7.2 g.

1. customThe solvent was removed under reduced pressure
2. additionthe residue diluted with ethyl acetate
3. washthis mixture was washed with saturated aqueous sodium chloride solution
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. customthe residue purified by column chromatography on silica gel
7. washeluting with a mixture of ethyl acetate and cyclohexane (1:4 by volume)