反应详情

To a solution of 0.264 g (1.654 mmol) of 4,5,6,7-tetrahydrofuro[2,3-c]pyridine hydrochloride, 0.41 g (1.8 mmol) of 4-benzoylbenzoic acid and 0.92 ml (6.6 mmol) of triethylamine in 30 ml of dichloromethane, 0.30 ml (2.0 mmol) of diethyl cyanophosphonate was added dropwise under ice-cooling, followed by overnight stirring at room temperature. This solution was poured into aqueous sodium hydroxide and extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous sodium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=3/1 to 2/1) to yield the desired product.

1. temperaturecooling
2. extractionextracted with dichloromethane 3 times
3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=3/1 to 2/1)