تفاعل #2358490
ord-acfe27147c714dbf9aa70e020235efe9
معادلة التفاعل
oxalyl chloride
5-(trifluoromethyl)benzo[b]thiophene-2-carboxylic acid
→
ethyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate
المردود 74.1%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةcooling
- 2درجة الحرارةunder reflux
- 3تركيزconcentrated under reduced pressure
- 4workup.ADDITIONTo the residue was added chloroform
- 5غسيلthe organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
- 6تجفيفdried over magnesium sulfate
- 7تركيزconcentrated under reduced pressure
الإجراء التجريبي
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).