反应详情

To a solution of 1-(3,5-bis-trifluoromethyl-benzoyl)-piperidin-4-one (5.1 g, 15 mmol) in acetic acid (20 mL) were added with cooling 3-chloroaniline (1.7 mL, 16.5 mmol) and trimethylsilylcyanide (1.9 mL, 15 mmol) so that the temperature did not rise above 20° C. The suspension was stirred for 6 h at room temperature. The reaction mixture was than added to ice-water (350 mL), ammonia (55 mL, 25%) was added to the mixture which was stirred for 15 min. After that the mixture was extracted with dichloromethane, the organic phases were pooled, washed with brine and dried with MgSO4. The solvent was evaporated and the residue crystallized from ethylacetate to yield the desired product (5.3 g, 74%), m.p. 205-207° C. and MS: m/e=476.1 (M+H+).

1. customdid not rise above 20° C
2. additionwas added to the mixture which
3. stirringwas stirred for 15 min
4. extractionAfter that the mixture was extracted with dichloromethane
5. washwashed with brine
6. dry with materialdried with MgSO4
7. customThe solvent was evaporated
8. customthe residue crystallized from ethylacetate