反应详情

In toluene, dissolved were 1-[3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]ethanone (10 g, 39 mmol) and DMFDMA (N,N-dimethyl formamide dimethyl acetal) (13.9 g, 117 mmol), and the mixture was heated under reflux. The reaction mixture was extracted with EA, and the extract was washed twice with brine, dried over MgSO4, filtered and evaporated under reduced pressure to remove solvent. The mixture was purified via column chromatography (MC/MeOH=10/1) to obtain 1-[3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]-3-(dimethylamino)prop-2-en-1-one (11 g, 92%).

1. temperaturethe mixture was heated
2. temperatureunder reflux
3. extractionThe reaction mixture was extracted with EA
4. washthe extract was washed twice with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customto remove solvent
9. customThe mixture was purified via column chromatography (MC/MeOH=10/1)