反应详情

Tri(o-toly)phosphine (9 mg, 0.030 mmol), palladium(II) acetate (6 mg, 0.027 mmol), methyl acrylate (31 mg, 0.34 mmol), triethylamine (116 mg, 1.14 mmol) and aryl bromide (32) (100 mg, 0.29 mmol) in acetonitrile (3 mL) were heated in a CEM Discover microwave for 90 minutes at 90° C. The solvent was removed under a stream of nitrogen gas, water was added and the organics extracted with EtOAc. The organic layer was dried (Na2SO4) and the solvent concentrated in vacuo. The crude product was purified by column chromatography eluting with 20% EtOAc in heptane. Yield: 41 mg, 40%; LC-MS tr 1.86 min; HPLC Purity: 67%; MS (ES+) m/z 356 (M+H)

1. customThe solvent was removed under a stream of nitrogen gas, water
2. additionwas added
3. extractionthe organics extracted with EtOAc
4. dry with materialThe organic layer was dried (Na2SO4)
5. concentrationthe solvent concentrated in vacuo
6. customThe crude product was purified by column chromatography
7. washeluting with 20% EtOAc in heptane