反应详情

温度

90 °C

To a solution of ethyl (2E)-3-(4-bromophenyl)acrylate (300 mg) in toluene (3 mL) was added palladium(II) acetate (26.4 mg), (R)-(+)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (110 mg), cesium carbonate (583 mg), and (3R)-1-(4-chlorobenzoyl)-3-pyrrolidinamine (291 mg). The mixture was heated at 90° C. for 2 days. The resulting mixture was poured into sat.NH4Cl aq solution and extracted with AcOEt. The organic layer was washed with sat. NH4Cl ag solution, water, and brine, and dried over Na2SO4. The solvent was removed in vacuo and residual brown oil was purified by preparative thin layer chromatography (chloroform methanol=95:5) to give ethyl (2E)-3-(4-{[(3R)-1-(4-chlorobenzoyl)-3-pyrrolidinyl]amino}phenyl)acrylate (297 mg) as pale yellow form.

1. additionThe resulting mixture was poured
2. extractionNH4Cl aq solution and extracted with AcOEt
3. washThe organic layer was washed with sat. NH4Cl ag solution, water, and brine
4. dry with materialdried over Na2SO4
5. customThe solvent was removed in vacuo and residual brown oil
6. customwas purified by preparative thin layer chromatography (chloroform methanol=95:5)