反应详情

A solution of 2-hydroxy-2-(3-nitrophenyl)acetonitrile (Preparation 113, 1.0 g, 5.62 mmol) in diethyl ether (10 ml) was stirred at room temperature and treated with pyridine (0.1 ml, 1.24 mmol) followed by thionyl chloride (0.82 ml, 11.2 mmol) dropwise over 5 minutes. The mixture was gently heated under reflux and after 30 min the solvent was removed by evaporation to give a pale yellow solid. This was purified by column chromatography on silica gel eluting with hexane:ethyl acetate (3:1 and then 2:1) to give the title compound as a white crystalline solid (980 mg, 89%).

1. temperatureThe mixture was gently heated
2. temperatureunder reflux and after 30 min the solvent
3. customwas removed by evaporation
4. customto give a pale yellow solid
5. customThis was purified by column chromatography on silica gel eluting with hexane:ethyl acetate (3:1