反应详情

温度

100 °C

Compound 7B (20 mg, 0.058 mmol), 4-bromobenzonitrile (16 mg, 0.088 mmol), tris(dibenzylideneacetone)dipallidium (2.1 mg, 0.0023 mmol), racemic-2,2′- bis(diphenylphosphino)-1,1′-binaphthyl (BINAP) (2.2 mg, 0.0035 mmol), cesium carbonate (29 mg, 0.088 mmol) and toluene (1 mL) were mixed and heated at 100° C. overnight. The reaction mixture was cooled, quenched with water, and extracted with dichloromethane 3×. Combined organic layer was dried over sodium sulfate, filtered and concentrated to give the crude product, which was then purified on silica gel column which was eluted with 0.3% ammonium hydroxide and 3% methanol in dichloromethane to give the desired product (12 mg, 46% yield).

1. temperatureThe reaction mixture was cooled
2. customquenched with water
3. extractionextracted with dichloromethane 3×
4. dry with materialCombined organic layer was dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customto give the crude product, which
8. customwas then purified on silica gel column which
9. washwas eluted with 0.3% ammonium hydroxide and 3% methanol in dichloromethane