반응 #2358485

반응 방정식

2-fluoro-5-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

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

수율 93.0%

용매

water

반응 조건

후처리

1. 1
   온도the reaction mixture was cooled to room temperature
2. 2
   추출extracted with tert-butyl methyl ether 3 times
3. 3
   세척The combined organic layer was washed with water
4. 4
   건조The mixture was dried over magnesium sulfate
5. 5
   농축concentrated under reduced pressure
6. 6
   기타The residue was recrystallized from methanol

실험 절차

A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60° C. for 2 hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 1).

출처