반응 #9738

반응 방정식

Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

intermediate 35

ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

sodium bromate

sodium bisulfite

→

title compound

{2-methyl-5-[4-(trifluoromethyl)phenyl]thien-3-yl}methanol

용매

cyclohexane

water

water

반응 조건

후처리

1. 1
   기타quenched with 1M sodium thiosulfate solution
2. 2
   추출extracted with ethyl acetate
3. 3
   세척washed with water, sodium thiosulfate
4. 4
   건조dried with brine and over MgSO4
5. 5
   농축concentrated

실험 절차

Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate (intermediate 35, 0.100 g) and sodium bromate (0.144 g) were suspended in a mixture of cyclohexane and water (1:1 v/v, 4 ml). To this was added a solution sodium bisulfite (0.99 g) in water (1 ml). The mixture was stirred for 2 hours, quenched with 1M sodium thiosulfate solution, then extracted with ethyl acetate. The organic layer was taken and washed with water, sodium thiosulfate and dried with brine and over MgSO4 and concentrated to give the title compound as a white crystalline solid.

출처