反応 #2358487

反応方程式

2-fluoro-6-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

methyl 4-(trifluoromethyl)benzo[b]thiophene-2-carboxylate

収率 35.4%

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

実験手順

A mixture of 1.00 g of 2-fluoro-6-(trifluoromethyl)benzaldehyde, 633 mg of methyl thioglycolate, 1.21 g of potassium carbonate and 15 ml of DMF was stirred at 130° C. for 2 hours. The reaction mixture was cooled to room temperature. To the reaction mixture was added water, and then 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 to obtain 480 mg of methyl 4-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 3).

出典