反応 #9734

反応方程式

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

溶媒

ethanol

反応条件

後処理

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

実験手順

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.

出典