HRID450855

反应详情

EQUATION

反应方程式

HRID 450855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of cyanothioacetamide (2.0 g, 20 mmol), the sodium salt of ethyl-3-oxo-butenol (2.44 g, 20 mmol) and piperidine acetate (1.9 ml) in water (20 ml) is heated at reflux before adding acetic acid (3 ml). The resulting precipitate is filtered and washed with water. The crude product is dissolved by heating in methanol. Filtering and evaporation of the solvent under reduced pressure yields 5,6-dimethyl-2-mercapto-nicotine nitrile.

WORKUP

后处理

  1. temperatureat reflux
  2. filtrationThe resulting precipitate is filtered
  3. washwashed with water
  4. dissolutionThe crude product is dissolved
  5. temperatureby heating in methanol
  6. filtrationFiltering
  7. customevaporation of the solvent under reduced pressure