反应详情

温度

60 °C

A solution of methyl 7-methoxy-3-oxoheptanoate (2.0 g) in methanol (70 ml) was cooled to 0° C.-5° C., 1-azido-2-chlorobenzene (1.08 g) and 28% sodium methoxide methanol solution (2 g) were added and the mixture was stirred at 60° C. for 3 hr. Then, 1N sodium hydroxide (14 ml) was added, and the mixture was stirred at 60° C. for 1 hr. The solvent was evaporated under reduced pressure and water (20 ml) was added to the residue. 1N Hydrochloric acid was added for neutralization and the mixture was extracted with ethyl acetate (50 ml×2). The extract was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate was concentrated under reduced pressure to give the object product (1.26 g) as a powder.

1. stirringthe mixture was stirred at 60° C. for 1 hr
2. customThe solvent was evaporated under reduced pressure and water (20 ml)
3. additionwas added to the residue
4. addition1N Hydrochloric acid was added for neutralization
5. extractionthe mixture was extracted with ethyl acetate (50 ml×2)
6. dry with materialThe extract was dried over anhydrous sodium sulfate
7. customthe solvent was evaporated under reduced pressure
8. washa fraction eluted with ethyl acetate
9. concentrationwas concentrated under reduced pressure