HRID1991451
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 2-cyano-3-thien-2-ylprop-2-enethioamide (4.2 g, 21 mmol), cycloheptone (2.4 g, 21 mmol) and piperidine (1.8 g, 22 mmol) in ethanol (100 mL) was heated to 80° C. overnight. After removal of the solvent, the residue was treated with water and extracted with ethyl acetate. The organic phase was washed with brine and dried over anhydrous sodium sulfate. The crude product, obtained after removal of the solvent, was purified by flash chromatography to afford 2-mercapto-4-thien-2-yl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carbonitrile (1.6 g, 25%).
WORKUP
后处理
- customAfter removal of the solvent
- additionthe residue was treated with water
- extractionextracted with ethyl acetate
- washThe organic phase was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customThe crude product, obtained
- customafter removal of the solvent
- customwas purified by flash chromatography