HRID550530

反应详情

EQUATION

反应方程式

HRID 550530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N,N′-dimethyl-5-hexenimidamide hydrochloride (3.1Mmol) in MeOH (20 ml) were added K2CO3 (3.1Mmol) and benzhydrazide (3.1Mmol). The solution was heated to reflux for 24 h. Volatiles were evaporated in vacuo, the crude dissolved in DCM, washed with water and dried over Na2SO4. After filtration and concentration to dryness in vacuo, the crude was purified by column chromatography (DCM:MeOH=98 to 2) to give 196 mg of the title compound.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureto reflux for 24 h
  3. customVolatiles were evaporated in vacuo
  4. dissolutionthe crude dissolved in DCM
  5. washwashed with water
  6. dry with materialdried over Na2SO4
  7. filtrationAfter filtration and concentration to dryness in vacuo
  8. customthe crude was purified by column chromatography (DCM:MeOH=98 to 2)