反应详情

温度

90 °C

To a stirred mixture of ethyl 3-(2-chlorophenyl)-2-(diethoxyphosphoryl)propanoate (step 1, 14.6 g, 41.9 mmol) and 37% formaldehyde in water (20 mL) was added a solution of potassium carbonate (17.4 g) in water (80 mL) at the room temperature and the mixture was stirred for 6 h at 90° C. After cooling to room temperature, the mixture was extracted with diethyl ether (300 mL), and then the organic layer washed with brine (100 mL), dried over magnesium sulfate, and evaporated. The residue was purified by column chromatography on silica gel (300 g) eluting with hexane/ethyl acetate (30/1) to afford 6.57 g (70%) of the title compound as a colorless oil:

1. temperatureAfter cooling to room temperature
2. extractionthe mixture was extracted with diethyl ether (300 mL)
3. washthe organic layer washed with brine (100 mL)
4. dry with materialdried over magnesium sulfate
5. customevaporated
6. customThe residue was purified by column chromatography on silica gel (300 g)
7. washeluting with hexane/ethyl acetate (30/1)