反应详情

Dichloromethane (85 mL) was added to Ph3P (4.942 g, 18.8 mmol), imidazole (1.311 g, 19.3 mmol) and I2 (4.735 g, 18.7 mmol). The mixture was stirred for 5 min. and then a solution of 12-2 (2.937 g, 15.0 mmol) in 15 mL dichloromethane was added by cannula. The reaction was stirred for 3 h, silica gel was added and the mixture evaporated. The residue was purified by flash chromatography on silica gel (10%→20%→30% ethyl acetate/hexanes) to give 12-3 (4.246 g, 13.9 mmol, 93%).

1. stirringThe reaction was stirred for 3 h
2. additionsilica gel was added
3. customthe mixture evaporated
4. customThe residue was purified by flash chromatography on silica gel (10%→20%→30% ethyl acetate/hexanes)