반응 #410858

반응 방정식

hydrochloric acid

2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenol

potassium carbonate

N,N-dimethylformamide

→

3,5-dichloro-4-(4-phthalimidobutyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene

수율 94.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   세척The ethyl acetate layer was successively washed with 10% hydrochloric acid and saturated saline solution
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   농축concentrated
4. 4
   기타to give crude crystals
5. 5
   세척The crude crystals were washed with n-hexane
6. 6
   기타dried under reduced pressure, which

실험 절차

A mixture of 9.1 g of 2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenol, 8.9 g of N-(4-bromoethyl)phthalimide, 4.4 g of potassium carbonate and 100 ml of N,N-dimethylformamide was stirred at room temperature for 24 hours. The reaction mixture was poured into ice water and made weak acidic by the addition of 10% hydrochloric acid, after which 200 ml of ethyl acetate was added for extraction. The ethyl acetate layer was successively washed with 10% hydrochloric acid and saturated saline solution, dried over anhydrous magnesium sulfate, and then concentrated to give crude crystals. The crude crystals were washed with n-hexane and then dried under reduced pressure, which afforded 14.5 g of 3,5-dichloro-4-(4-phthalimidobutyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene (94% yield).

출처