反应 #9734

反应方程式

ethyl thioglycolate

Sodium hydride

N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate

intermediate 34

N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate

→

title compound

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

溶剂

ethanol

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   浓缩The cooled mixture was concentrated in vacuo
3. 3
   其他the residue partitioned between water and diethyl ether
4. 4
   其他The organic layer was collected
5. 5
   干燥dried over magnesium sulphate
6. 6
   浓缩concentrated

实验过程

Sodium hydride (60% dispersion in mineral oil, 0.528 g) was added to dry ethanol (20 ml), N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate (intermediate 34, 2.8 g) was added followed by ethyl thioglycolate (0.79 g) and the mixture heated at 110° C. for 2 hours under nitrogen. The cooled mixture was concentrated in vacuo and the residue partitioned between water and diethyl ether. The organic layer was collected, dried over magnesium sulphate and concentrated to give the title compound as a brown solid.

来源