反应 #417928

反应方程式

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

tetrahydrofurane

HCl

→

colourless crystals

收率 37.3%

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

收率 37.3%

溶剂

ethylacetate cyclohexane

反应条件

后处理

1. 1
   workup.ADDITIONdiluted with methylenehloride
2. 2
   萃取extracted
3. 3
   干燥The organic phase was dried with sodiumsulfate
4. 4
   浓缩concentrated

实验过程

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).

来源