反应详情

温度

65 °C

A mixture of 2,4-difluoro-benzoic acid tert-butyl ester (30 g, 140.05 mmol) and (R)-2-methoxy-1-methyl-ethylamine (100 mL) was stirred at 65° C. for 2 days. A satured solution of NaHCO3 was added and the mixture was extracted with dichloromethane (3 times). The organic phase was washed twice with water then with brine, dried over sodium sulfate filtered and evaporated to dryness to obtain a crude, which was purified by column chromatography on silica gel (exane/ethyl acetate 9:1). The title compound (33.38 g, 84%) was obtained as oil.

1. extractionthe mixture was extracted with dichloromethane (3 times)
2. washThe organic phase was washed twice with water
3. dry with materialwith brine, dried over sodium sulfate
4. filtrationfiltered
5. customevaporated to dryness
6. customto obtain a crude, which
7. customwas purified by column chromatography on silica gel (exane/ethyl acetate 9:1)