반응 #4862

반응 방정식

2-bromo-m-xylene

N-allylphthalimide

acetate

triphenylphosphine

→

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

용매

triethylamine

ether

water

반응 조건

후처리

1. 1
   기타The aqueous layer was separated
2. 2
   세척the organic washed twice with 100 ml portions of 2N HCl
3. 3
   여과After filtering the organic phase
4. 4
   세척washing with saturated KHCO3 and brine
5. 5
   건조drying over MgSO4, it
6. 6
   농축was concentrated on the steam bath
7. 7
   기타The resulting solid product was purified by flash chromotography

실험 절차

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.

출처