反应 #2358485

反应方程式

2-fluoro-5-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

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

收率 93.0%

溶剂

water

反应条件

后处理

1. 1
   温度the reaction mixture was cooled to room temperature
2. 2
   萃取extracted with tert-butyl methyl ether 3 times
3. 3
   洗涤The combined organic layer was washed with water
4. 4
   干燥The mixture was dried over magnesium sulfate
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他The residue was recrystallized from methanol

实验过程

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).

来源