反応 #417927

反応方程式

ethylacetate cyclohexane

thioacetic acid S-(2-trifluoromethyl-benzyl)ester

methanol

3-Bromomethyl-pyridine-2-carboxylic acid methyl ester

→

colorless crystals

収率 100.0%

3-(2-Trifluoromethyl-benzylsulfanylmethyl)-pyridine-2-carboxylic acid methyl ester

収率 100.0%

溶媒

water

反応条件

後処理

1. 1
   温度after refluxing for 150 min the solution
2. 2
   抽出extracted with ethylacetate
3. 3
   乾燥the organic phase dried with sodium sulfate
4. 4
   濃縮concentrated

実験手順

To a solution of thioacetic acid S-(2-trifluoromethyl-benzyl)ester (10.2 g, 37.5 mmol) in methanol (130 ml) potassium carbonate (5.18 g, 37.5 mmol) was added at room temperature and it was stirred for 30 min. 3-Bromomethyl-pyridine-2-carboxylic acid methyl ester (4.40 g, 18.7 mmol) was added and after refluxing for 150 min the solution was diluted with water, extracted with ethylacetate, the organic phase dried with sodium sulfate and concentrated. Chromatography over silica with ethylacetate/cyclohexane gave 7.82 g colorless crystals (18.7 mmol).

出典