반응 #458623

반응 방정식

N,N-dimethylformamide

3-phenoxy-α-cyanobenzyl cis-2,2-dimethyl-3-(2,2,2-trichloroethyl)cyclopropanecarboxylate

triethanolamine

hydrogen sulfide

→

3-phenoxy-α-thiocarbamoylbenzyl cis-2,2-dimethyl-3-(2,2,2-trichloroethyl)cyclopropanecarboxylate

수율 98.0%

용매

water

반응 조건

후처리

1. 1
   기타was bubbled into the solution at room temperature over a period of 15 hours
2. 2
   기타The resultant reaction mixture
3. 3
   추출extracted with diethyl ether
4. 4
   세척The ethereal layer was washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONdistilled
7. 7
   기타to remove diethyl ether

실험 절차

Into 20 ml of N,N-dimethylformamide were dissolved 2.50 g of 3-phenoxy-α-cyanobenzyl cis-2,2-dimethyl-3-(2,2,2-trichloroethyl)cyclopropanecarboxylate and 1 ml of triethanolamine, and hydrogen sulfide gas was bubbled into the solution at room temperature over a period of 15 hours. The resultant reaction mixture was poured into 500 ml of water and extracted with diethyl ether. The ethereal layer was washed with water, dried over anhydrous magnesium sulfate and distilled to remove diethyl ether. By the above procedure there were obtained 2.63 g of 3-phenoxy-α-thiocarbamoylbenzyl cis-2,2-dimethyl-3-(2,2,2-trichloroethyl)cyclopropanecarboxylate [Compound (27)] having the NMR spectrum shown hereinbelow (yield: 98%)

출처