反应详情

温度

100 °C

To a solution of 0.230 g (0.694 mmol) of 5-(4-benzoylbenzoyl)-4,5,6,7-tetrahydrofuro[3,2-c]pyridine in 20 ml of acetic acid, 0.094 ml (1.04 mmol) of 50% aqueous dimethylamine and 0.085 ml (1.04 mmol) of 37% aqueous formaldehyde were added, followed by stirring at 100° C. for 1 hour. After the solvent was distilled off under reduced pressure, the residual solution was alkalified with 5% aqueous sodium hydrogen carbonate and extracted with dichloromethane 2 times. The combined organic layer was washed with water and dried over anhydrous sodium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (chloroform to chloroform/methanol=50/1); the resulting solid was washed with hexane to yield the desired product.

1. distillationAfter the solvent was distilled off under reduced pressure
2. extractionextracted with dichloromethane 2 times
3. washThe combined organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe resulting crude product was purified by silica gel column chromatography (chloroform to chloroform/methanol=50/1)
7. washthe resulting solid was washed with hexane