반응 #75565

반응 방정식

2-[2-(5-Bromo-2-methoxy-phenyl)-ethyl]-3-chloro-thiobenzamide

hydrogen sulfide

2-[2-(5-Bromo-2-methoxy-phenyl)-ethyl]-3-chloro-benzonitrile

→

crude product

2-[2-(5-Bromo-2-methoxy-phenylsulfanylmethyl)-phenyl]-1,4,5,6-tetrahydro-pyrimidine

용매

water

ethanol

triethylamine

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate twice
2. 2
   세척The organic extracts were washed with brine
3. 3
   건조dried (MgSO4)
4. 4
   여과filtered
5. 5
   기타evaporated

실험 절차

9, 2-[2-(5-Bromo-2-methoxy-phenyl)-ethyl]-3-chloro-thiobenzamide. As shown in Scheme 9, hydrogen sulfide gas was bubbled into a solution of 2.75 g (7.8 mmol) of 2-[2-(5-Bromo-2-methoxy-phenyl)-ethyl]-3-chloro-benzonitrile in 20 mL of ethanol and triethylamine (5:4 v/v) for 10 minutes. The solution was then heated to 80° C. in a sealed pressure tube for 5 hours. The reaction mixture was diluted with water and extracted with ethyl acetate twice. The organic extracts were washed with brine, dried (MgSO4), filtered and evaporated to give 3.0 g of crude product which was used directly in the next step.

출처