反应详情

温度

140 °C

18.8 g (82 mmol) of ethyl 2-bromobenzoate, 17.2 g (107 mmol) of 4-(N,N,-dimethylaminomethyl)styrene [sic], 20.7 g (205 mmol) of triethylamine, 0.36 g of palladium(II) acetate and 0.96 g of tri(o-tolyl)phosphine were mixed in 200 ml of dimethylformamide and, after addition of 1 ml of water, stirred at 140° C. for 3 h. The reaction mixture was then concentrated in vacuo, and the resulting residue was partitioned between ethyl acetate and water. The organic phase was separated off, washed with water, dried and concentrated in vacuo. The residue was then recrystallized from petroleum ether. 16.1 g (63%) of the product were obtained.

1. concentrationThe reaction mixture was then concentrated in vacuo
2. customthe resulting residue was partitioned between ethyl acetate and water
3. customThe organic phase was separated off
4. washwashed with water
5. customdried
6. concentrationconcentrated in vacuo
7. customThe residue was then recrystallized from petroleum ether