反应 #4862

反应方程式

2-bromo-m-xylene

N-allylphthalimide

acetate

triphenylphosphine

→

2-[3-(2,6-dimethylphenyl)-2-propenyl]-1H-isoindole-1,3(2H)-dione

溶剂

triethylamine

ether

water

反应条件

后处理

1. 1
   其他The aqueous layer was separated
2. 2
   洗涤the organic washed twice with 100 ml portions of 2N HCl
3. 3
   过滤After filtering the organic phase
4. 4
   洗涤washing with saturated KHCO3 and brine
5. 5
   干燥drying over MgSO4, it
6. 6
   浓缩was concentrated on the steam bath
7. 7
   其他The resulting solid product was purified by flash chromotography

实验过程

A mixture 9.3 g (50 mmole) of 2-bromo-m-xylene, 15.0 g (80 mmole) of N-allylphthalimide, 0.56 (2.5 mmole) of paladium acetate and 1.44 (5.5 mmole) of triphenylphosphine were dissolved in 111 ml of triethylamine. The solution was placed in a sealed container and heated at 100° C. for 24 hours. The reaction was then diluted with 800 ml of ether and 200 ml of water. The aqueous layer was separated and the organic washed twice with 100 ml portions of 2N HCl. After filtering the organic phase, washing with saturated KHCO3 and brine, and drying over MgSO4, it was concentrated on the steam bath. The resulting solid product was purified by flash chromotography and used in subsequent reactions.

来源