HRID1107358

反应详情

EQUATION

反应方程式

HRID 1107358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a similar manner to Example 85 reaction of 3-methylthio-5-chloro-6-carboethoxy-1,2,4-triazine (prepared from 3-methylthio-5-oxo-6-carboethoxy-4,5-dihydro-1,2,4-triazine, 1.5 g) with 2-isobutoxybenzamidine hydrochloride (2.37 g) and triethylamine (1.75 g) afforded the crude title compound (1.71 g). This was recrystallized from acetonitrile, then dissolved in chloroform, the organic solution was washed with 2 Normal hydrochloric acid (x2), chloroform removed under reduced pressure and the residue recrystallized twice from ethanol to afford the title compound, 0.32 g, m.p. 237-238° C.

WORKUP

后处理

  1. customafforded the crude title compound (1.71 g)
  2. customThis was recrystallized from acetonitrile
  3. dissolutiondissolved in chloroform
  4. washthe organic solution was washed with 2 Normal hydrochloric acid (x2), chloroform
  5. customremoved under reduced pressure
  6. customthe residue recrystallized twice from ethanol