反应详情

A mixture of 2-(4-Bromo-phenyl)-2-hydroxy-N-(4-trifluoromethyl-phenyl)-acetamide (8.0 g, 21.4 mmol), (2-acryloylamino-phenyl)-carbamic acid tert-butyl ester (6.2 g, 23.6 mmol), tri-o-tolyl-phosphine (1.0 g, 3.3 mmol), triethylamine (12 mL, 86 mmol), and Pd2(dba)3 (1.5 g, 1.6 mmol) in DMF (160 mL) was heated at 90 degrees Celcius overnight under nitrogen atmosphere. The mixture was poured into saturated ammonium chloride solution (300 mL) and extracted with ethyl acetate three times. The organic layer was washed with brine, dried over sodium sulfate, filtered, concentrated, and purified by flash column chromatography (ethyl acetate/petroleum ether 1:2) to obtain a white solid (5.8 g, 49%).

1. temperaturewas heated at 90 degrees Celcius overnight under nitrogen atmosphere
2. extractionextracted with ethyl acetate three times
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by flash column chromatography (ethyl acetate/petroleum ether 1:2)