反応 #417928

反応方程式

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

tetrahydrofurane

HCl

→

colourless crystals

収率 37.3%

6,6-Dioxo-7-(2-trifluoromethyl-phenyl)-5,6-dihydro-thiopyrano[4,3-b]pyridin-8-ol

収率 37.3%

溶媒

ethylacetate cyclohexane

反応条件

後処理

1. 1
   workup.ADDITIONdiluted with methylenehloride
2. 2
   抽出extracted
3. 3
   乾燥The organic phase was dried with sodiumsulfate
4. 4
   濃縮concentrated

実験手順

To a solution of 3-(2-Trifluoromethyl-phenylmethanesulfonylmethyl)-pyridine-2-carboxylic acid methyl ester (7.58 g, 19.6 mmol) in tetrahydrofurane (160 ml) potassium tert-butoxide (2.20 g, 19.57 mmol) was added at room temperature and stirring was continued for 3.5 h. 1M HCl was added, diluted with methylenehloride and extracted. The organic phase was dried with sodiumsulfate and concentrated. Chromatography over silica with ethylacetate/cyclohexane gave 2.50 g colourless crystals (7.32 mmol).

出典