تفاعل #9734

معادلة التفاعل

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

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   تركيزThe cooled mixture was concentrated in vacuo
3. 3
   أخرىthe residue partitioned between water and diethyl ether
4. 4
   أخرىThe organic layer was collected
5. 5
   تجفيفdried over magnesium sulphate
6. 6
   تركيزconcentrated

الإجراء التجريبي

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.

المصدر