反应详情

温度

80 °C

Under a nitrogen atmosphere a mixture of 40.0 g (137 mmol) 2-benzyloxy-5-bromo-1,3-dimethylbenzene and 24.1 g (165 mmol) methyl 2-acetylamino-acrylate in 420 mL triethylamine and 200 mL acetonitrile was combined with 3.5 g (11.2 mmol) tri-o-tolyl-phosphane and 2.5 g (11.1 mmol) Pd(OAc)2 and stirred for 18 h at 80° C. The precipitate was suction filtered, the filtrate concentrated by evaporation i.vac. and combined with 800 mL DCM and 800 mL water. The organic phase was separated off, suction filtered on Na2SO4, the solvent was eliminated i.vac., the residue was stirred with EtOAc, suction filtered and dried i.vac.

1. filtrationfiltered
2. concentrationthe filtrate concentrated by evaporation i.vac
3. customThe organic phase was separated off
4. filtrationsuction filtered on Na2SO4
5. stirring, the residue was stirred with EtOAc, suction
6. filtrationfiltered
7. customdried i.vac