반응 #2358490

반응 방정식

oxalyl chloride

5-(trifluoromethyl)benzo[b]thiophene-2-carboxylic acid

→

ethyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate

수율 74.1%

용매

ethanol

반응 조건

후처리

1. 1
   온도cooling
2. 2
   온도under reflux
3. 3
   농축concentrated under reduced pressure
4. 4
   workup.ADDITIONTo the residue was added chloroform
5. 5
   세척the organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
6. 6
   건조dried over magnesium sulfate
7. 7
   농축concentrated under reduced pressure

실험 절차

Then, 254 mg of oxalyl chloride was added to a mixture of 400 mg of 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylic acid and 20 ml of ethanol while ice-cooling, and the mixture was stirred for 6 hours under reflux. The reaction mixture was cooled to room temperature, and then concentrated under reduced pressure. To the residue was added chloroform, and then the organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure to obtain 330 mg of ethyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 5).

출처