反応 #9738

反応方程式

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

溶媒

cyclohexane

water

water

反応条件

後処理

1. 1
   その他quenched with 1M sodium thiosulfate solution
2. 2
   抽出extracted with ethyl acetate
3. 3
   洗浄washed with water, sodium thiosulfate
4. 4
   乾燥dried with brine and over MgSO4
5. 5
   濃縮concentrated

実験手順

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.

出典