反応 #2358485

反応方程式

2-fluoro-5-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

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

収率 93.0%

溶媒

water

反応条件

後処理

1. 1
   温度the reaction mixture was cooled to room temperature
2. 2
   抽出extracted with tert-butyl methyl ether 3 times
3. 3
   洗浄The combined organic layer was washed with water
4. 4
   乾燥The mixture was dried over magnesium sulfate
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他The residue was recrystallized from methanol

実験手順

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).

出典