反应详情

2,2,2-trichloro-N-(4-chloro-3-(trifluoromethyl)phenyl)acetamide (45 g, 0.1319 mol) was refluxed in N,N-dimethyl formamide (100 ml) with 1,8-diazabicyclo[5.4.0]undec-7-ene (24.67 ml, 0.1649 mol) and 4-(4-aminophenoxy)-N-methylpicolinamide (32.07 g, 0.1319 mol) for 24 hours and cooled to room temperature. The reaction mass was quenched in water (1000 ml). The quenched mass was extracted repeatedly with ethyl acetate and the combined ethyl acetate layer was then back washed with water to remove DMF traces. It was dried over sodium sulfate and evaporated under vacuum to obtain solid. The obtained solid was slurried in ethyl acetate (1000 ml) at ambient temperature and filtered to give 4-(4-(3-(4-chloro-3-(trifluoromethyl)phenyl) ureido)phenoxy)-N-methylpicolinamide (sorafenib base) (52 g).

1. customThe reaction mass was quenched in water (1000 ml)
2. extractionThe quenched mass was extracted repeatedly with ethyl acetate
3. washthe combined ethyl acetate layer was then back washed with water
4. customto remove DMF traces
5. dry with materialIt was dried over sodium sulfate
6. customevaporated under vacuum
7. customto obtain solid
8. filtrationfiltered