反应详情

温度

200 °C

A solution of N-[4-chloro-2-methyl-3-(trifluoromethyl)phenyl]-2,2-dimethylpropanamide (0.257 g, 0.875 mmol) in NMP (2.5 mL) was treated with copper cyanide (0.180 g, 2.01 mmol) and the resulting suspension was heated to 200° C. in a microwave for 14 h. The cooled reaction mixture was diluted with EtOAc and water and then filtered through a pad of celite. The filtrate was concentrated to a brown oil and then partitioned between Et2O and water. The aqueous portion was further extracted with Et2O and the combined organics were dried (Na2SO4), filtered, and concentrated to a brown foam. Trituration with hexanes/Et2O afforded the title compound (0.222 g) in good purity: MS (ES) m/z 285 (M+1).

1. customThe cooled reaction mixture
2. filtrationfiltered through a pad of celite
3. concentrationThe filtrate was concentrated to a brown oil
4. custompartitioned between Et2O and water
5. extractionThe aqueous portion was further extracted with Et2O
6. dry with materialthe combined organics were dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated to a brown foam