HRID1991451

反应详情

EQUATION

反应方程式

HRID 1991451 反应方程式

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

  1. customAfter removal of the solvent
  2. additionthe residue was treated with water
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe crude product, obtained
  7. customafter removal of the solvent
  8. customwas purified by flash chromatography