HRID258745

反应详情

EQUATION

反应方程式

HRID 258745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of the isothiourea dihydrochloride of Example 1 (i) (6.7 g), N-methyl-N-tert-butoxycarbonylhydrazine sulphate (5.7 g), potassium hydrogen carbonate (10.0 g) and anhydrous dimethylformamide (80 ml) was stirred at 90° C. for 3 hours. After cooling, filtration and concentration to yield the free base, this was heated under reflux with ethanolic hydrogen chloride. Concentration and trituration of the residual product yielded the title compound.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationfiltration and concentration
  3. customto yield the free base
  4. temperaturethis was heated
  5. concentrationConcentration and trituration of the residual product