反应详情

温度

120 °C

To a solution of 4-chloro-N,N-diethyl-2-(trifluoromethyl)benzamide (5.04 g, 18 mmol) in 100 mL of N,N-dimethylformamide was added potassium carbonate (6.2 g, 45 mmol) and diethylzinc (29.5 mL of a 1.1 M solution in toluene, 32.4 mmol). The mixture was degassed and then there was added POPd (Combiphos) (0.27 g, 0.54 mmol). The resulting solution was heated at 120° C. in a sealed tube for 18 h. The mixture was allowed to cool and was diluted with water and extracted with ethyl acetate. The organics were washed with water and brine, dried (MgSO4) and concnentrated in vacuo. The residue was purified (ISCO, elution with 0-25% EtOAc/hexane) to afford 3.7 g (75%) of the title compound as an oil. LRMS (ESI): 274.2 (M+H)+.

1. customThe mixture was degassed
2. additionthere was added POPd (Combiphos) (0.27 g, 0.54 mmol)
3. temperatureto cool
4. additionwas diluted with water
5. extractionextracted with ethyl acetate
6. washThe organics were washed with water and brine
7. dry with materialdried (MgSO4)
8. customThe residue was purified
9. wash(ISCO, elution with 0-25% EtOAc/hexane)