反应详情

温度

100 °C

To a solution of 0.341 g (1.029 mmol) of 6-(4-benzoylbenzoyl)-4,5,6,7-tetrahydrofuro[2,3-c]pyridine in 10 ml of acetic acid, 0.18 g (1.2 mmol) of N-methyl-2-methoxyethylammonium acetate and 0.10 g (1.2 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 aqueous sodium hydroxide and 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 column chromatography (ethyl acetate to ethyl acetate/methanol=4/1) to yield the desired product.

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