反应详情

To 30 ml of N,N-dimethylformamide, 0.33 ml (3.6 mmol) of phosphorus oxychloride was added under ice-cooling, followed by stirring at room temperature for 0.5 hours. To this mixture, a solution of 1.064 g (3.578 mmol) of 1-(5,7-dihydro-4H-furo[2,3-c]pyridin-6-yl)-6-phenylhexan-1-one in 20 ml of N,N-dimethylformamide was added, followed by overnight stirring at room temperature. After water was added, the reaction mixture was extracted with ethyl acetate 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel flush column chromatography (hexane/ethyl acetate=2/1 to 1/1) to yield the desired product.

1. temperaturecooling
2. waitfollowed by overnight
3. stirringstirring at room temperature
4. extractionthe reaction mixture was extracted with ethyl acetate 3 times
5. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe resulting crude product was purified by silica gel
8. customflush column chromatography (hexane/ethyl acetate=2/1 to 1/1)