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 (S)-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×). The organic phase was washed with water (2×), brine, dried over sodium sulfate filtered and evaporated to dryness to obtain a crude, which was purified by column chromatography on silica gel (exane-EtOAc 9:1). The title compound (33.38 g, 84%) was obtained as oil.

1. extractionthe mixture was extracted with dichloromethane (3×)
2. washThe organic phase was washed with water (2×), brine
3. dry with materialdried 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-EtOAc 9:1)