反应详情

温度

0 °C

To a solution of 4-chloro-2-(ethoxycarbonylamino)benzonitrile (10.8 g) in DMF (50 ml) cooled to 0° C. was added sodium hydride (60% w/w dispersion in mineral oil, 2.0 g, 50 mmol). The mixture was stirred for 30 min at 0° C. and then 2-bromoacetophenone (9.9 g, 50 mmol) was carefully added. After stirring for an additional 15 h at 0° C., the mixture was poured into water (500 ml) and extracted with diethyl ether (500 ml×2). After drying (MgSO4) and removal of solvent, the crude product was purified by flash chromatography eluting with ethyl acetate/hexane (1:5) to afford 11.8 g (72%) of the title compound as a brown amorphous solid.

1. stirringAfter stirring for an additional 15 h at 0° C.
2. extractionextracted with diethyl ether (500 ml×2)
3. customAfter drying
4. custom(MgSO4) and removal of solvent
5. customthe crude product was purified by flash chromatography
6. washeluting with ethyl acetate/hexane (1:5)