反应 #9738

反应方程式

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

溶剂

cyclohexane

water

water

反应条件

后处理

1. 1
   其他quenched with 1M sodium thiosulfate solution
2. 2
   萃取extracted with ethyl acetate
3. 3
   洗涤washed with water, sodium thiosulfate
4. 4
   干燥dried with brine and over MgSO4
5. 5
   浓缩concentrated

实验过程

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.

来源