反应 #1265373

反应方程式

water

ethyl 2-bromobenzoate

4-(N,N,-dimethylaminomethyl)styrene

triethylamine

→

product

收率 63.5%

Ethyl 2-(E-2-(4-(N,N-dimethylaminomethyl)phenyl)ethen-1-yl)benzoate

收率 63.5%

溶剂

dimethylformamide

反应条件

后处理

1. 1
   浓缩The reaction mixture was then concentrated in vacuo
2. 2
   其他the resulting residue was partitioned between ethyl acetate and water
3. 3
   其他The organic phase was separated off
4. 4
   洗涤washed with water
5. 5
   其他dried
6. 6
   浓缩concentrated in vacuo
7. 7
   其他The residue was then recrystallized from petroleum ether

实验过程

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.

来源