HRID235662

反应详情

EQUATION

反应方程式

HRID 235662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 3,4-dimethoxy-1,2,5-thiadiazole-1-oxide (1.62 g) in methanol was reacted with a solution of 4-(5-bromo-3-methylpyrid-2-yl)-butylamine (2.43 g) in methanol. After 2 hours at room temperature, the reaction was cooled to 0° C. and saturated by passing ammonia gas for 10 mins. After 1.5 hours the product (which precipitated) was filtered off and recrystallised from ethanol to yield 3-[4-(5-bromo-3-methylpyrid-2-yl)-butylamino]-4-amino-1,2,5-thiadiazole-1-oxide (1.12 g) m.p. 188°-190° C.

WORKUP

后处理

  1. customfor 10 mins
  2. customAfter 1.5 hours the product (which precipitated)
  3. filtrationwas filtered off
  4. customrecrystallised from ethanol