反应详情

温度

5 °C

A mixture of intermediate 11 (0.0536 mol) in DCM (200 ml) was cooled to 5° C. under N2 flow. A solution of trichloro-acetylchloride (0.0643 mol) was added dropwise at 5° C. The mixture was stirred at 5° C. for 30 minutes. A solution of triethylamine (0.0643 mol) was added dropwise at 5° C. The mixture was stirred at 5° C. for 1 hour then at room temperature for 2 hours, poured out into ice water and extracted with DCM. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated, yielding 27.4 g (quantitative) of 2,2,2-trichloro-N-[2-(3-chlorobenzoyl)-4-(4-methoxybenzoyl)phenyl]-acetamide (intermediate 12).

1. stirringThe mixture was stirred at 5° C. for 1 hour
2. waitat room temperature for 2 hours
3. extractionextracted with DCM
4. customThe organic layer was separated
5. washwashed with water
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customthe solvent was evaporated