HRID1730879

反应详情

EQUATION

反应方程式

HRID 1730879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.5 g. of 6-chloro-1,2,4-triazolo[4,3-b]pyridazin-3(2H)-one (0.12 mol.) and a solution of 14.85 g. of methylamine (0.48 mol.) in 160 ml. of benzene are heated in an autoclave at 120° for 5 hours. After cooling, the precipitated product is filtered off and the filtrate is evaporated to dryness. Both portions of 6-methylamino-1,2,4-triazolo[4,3-b]pyridazin-3(2H)-one are treated with dilute aqueous hydrochloric acid, filtered off and recrystallized from water to give 15.8 g. (80%) of material, m.p. > 348° .

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe precipitated product is filtered off
  3. customthe filtrate is evaporated to dryness
  4. additionBoth portions of 6-methylamino-1,2,4-triazolo[4,3-b]pyridazin-3(2H)-one are treated with dilute aqueous hydrochloric acid
  5. filtrationfiltered off
  6. customrecrystallized from water
  7. customto give 15.8 g