反应详情

To a solution of tert-butyl 2-(6-(4-bromophenyl)pyridin-3-yl)propan-2-ylcarbamate, 33-f, (850 mg, 2.17 mmol) in toluene (15 ml) was added diethyl phosphonate (900 mg, 6.52 mmol) and Et3N (660 mg, 6.52 mmol) and PdCl2(dppf) (85 mg) under N2, and the reaction mixture was refluxed for 8 hours. The reaction solution was then evaporated and diluted with EtOAc. The organic phase was washed with brine, dried and concentrated. Purified by silica gel (DCM-DCM:MeOH=50:1) to give tert-butyl 2-(6-(4-(diethoxyphosphoryl)phenyl)pyridin-3-yl)propan-2-ylcarbamate (900 mg, 92.4%).

1. temperaturethe reaction mixture was refluxed for 8 hours
2. customThe reaction solution was then evaporated
3. additiondiluted with EtOAc
4. washThe organic phase was washed with brine
5. customdried
6. concentrationconcentrated
7. customPurified by silica gel (DCM-DCM:MeOH=50:1)