反応 #417929

反応方程式

water

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

pyridine

pivaloylchloride

→

colourless crystals

収率 15.7%

2,2-Dimethyl-propionic acid 6,6-dioxo-7-(2-trifluoromethyl-phenyl)-5,6-dihydro-thiopyrano[4,3-b]pyridin-8-yl ester

収率 15.7%

溶媒

ethylacetate cyclohexane

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   その他the organic phase separated
3. 3
   濃縮concentrated

実験手順

To a solution of 6,6-Dioxo-7-(2-trifluoromethyl-phenyl)-5,6-dihydro-thiopyrano[4,3-b]pyridin-8-ol (1.92 g, 5.61 mmol) prepared according to the above Example 1 in methylenehloride (70 ml) was added at 0° C. pyridine (1.77 g, 22.4 mmol), followed by pivaloylchloride (0.744 g, 6.17 mmol). After stirring at room temperature for 16 h methylenehloride and water was added, the organic phase separated and concentrated. Chromatography over silica with ethylacetate/cyclohexane gave 380 mg colourless crystals (0.88 mmol).

出典