反应详情

温度

-78 °C

A solution of 7-methoxyfuro[2,3-c]pyridine (1.5 g) in dry tetrahydrofuran (50 ml) was stirred at −78° C. under dry nitrogen. n-Butyllithium (1.6N solution in hexanes, 6.9 ml) was added dropwise and the resulting solution stirred at −78° C. for 60 minutes. Acetaldehyde (5.7 ml) was added and stirring continued at −78° C. for 90 minutes before warming to room temperature. The mixture was diluted with water (100 ml) and extracted with ethyl acetate (3×100 ml). The combined organic extracts were dried over magnesium sulfate, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 50% hexane in ethyl acetate gave the title compound (1.8 g) as a brown oil.

1. stirringstirring
2. waitcontinued at −78° C. for 90 minutes
3. temperaturebefore warming to room temperature
4. extractionextracted with ethyl acetate (3×100 ml)
5. dry with materialThe combined organic extracts were dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent removed in vacuo
8. customPurification by column chromatography on silica eluting with 50% hexane in ethyl acetate