HRID464284

反应详情

EQUATION

反应方程式

HRID 464284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chloro-[1,2,4]triazolo-[4,3-a]quinoxaline (2.0 g., 0.01 mole), the product of Example 2, in N,N-dimethyl formamide (30 ml.) was saturated with monomethylamine gas and stirred at room temperature for 3 hours. Monomethylamine gas was again bubbled into the solution and the solution was stirred at room temperature for an additional 2 hours. The precipitate was separated by filtration and washed with N,N-dimethylformamide. Recrystallization from N,N-dimethylformamide gave 1.37 g. (69% yield) of 4-methylamino-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. >300° C. Mass spectrum: m/e, 199 (P).

WORKUP

后处理

  1. customMonomethylamine gas was again bubbled into the solution
  2. stirringthe solution was stirred at room temperature for an additional 2 hours
  3. customThe precipitate was separated by filtration
  4. washwashed with N,N-dimethylformamide
  5. customRecrystallization from N,N-dimethylformamide
  6. customgave 1.37 g