反应详情

温度

150 °C

A mixture of 4.50 g (13.2 mmol) of methyl 3-(3,5-dichloropyridin-2-yl)-2-(2-fluorophenyl)-3-oxopropanoate from example 1A, 845 mg (14.5 mmol) of sodium chloride, 474 mg (26.3 mmol) of water and 13.5 ml of DMSO is heated in a microwave at 150° C. for 10 min and then stirred into water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated. The residue is purified by chromatography on silica gel (eluent: dichloromethane) to result in a yellow oil which gradually crystallizes and affords 3.18 g (85% of theory) of the title compound.

1. extractionextracted with ethyl acetate
2. dry with materialThe organic phase is dried over sodium sulfate
3. concentrationconcentrated
4. customThe residue is purified by chromatography on silica gel (eluent: dichloromethane)
5. customto result in a yellow oil which
6. customgradually crystallizes