反应详情

温度

60 °C

To a solution of 2-chloro-N-(1H-indazol-6-yl)-5-iodo-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.45 g, 0.8 mmol) in dimethylformamide (2.0 mL) was added tetravinyltin (0.29 mL, 1.6 mmol) and tetrakis(triphenylphosphine)palladium(0) (Pd(PPh3)4) (0.092 g, 0.08 mmol). After degassing, the mixture was heated at 60° C. for 15 h. before it was diluted with EtOAc, and washed sequentially with Sat. NaHCO3 and brine. The organic extract was dried over Na2SO4 and concentrated to give a crude residue. Purification by flash column chromatography (Hexane/EtOAc=1:1) gave 2-chloro-N-(1H-indazol-6-yl)-5-vinyl-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.11 g).

1. customAfter degassing
2. additionwas diluted with EtOAc
3. washwashed sequentially with Sat. NaHCO3 and brine
4. extractionThe organic extract
5. dry with materialwas dried over Na2SO4
6. concentrationconcentrated
7. customto give a crude residue
8. customPurification by flash column chromatography (Hexane/EtOAc=1:1)