HRID1065104

反应详情

EQUATION

反应方程式

HRID 1065104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

48.6 g (0.243 mol) of 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5(4H)-one (V) were introduced into a mixture of 236 g of 45% strength sodium hydroxide solution and 160 g of water, while stirring. When all of the product had dissolved, 40.2 g of methyl iodide were added in a manner such that the internal temperature did not exceed 30° C. When the addition had ended, the reaction mixture was stirred at room temperature for a further 2 hours. The reaction product which had precipitated was then filtered off, washed with 100 ml of water and dried. 42.5 g (82% of theory) of 4-amino-6-tert.-butyl-3-methylthio-1,2,4-triazin-5(4H)-one (I) of melting point 123°-125° C. were obtained.

WORKUP

后处理

  1. dissolutionWhen all of the product had dissolved
  2. customdid not exceed 30° C
  3. additionWhen the addition
  4. stirringthe reaction mixture was stirred at room temperature for a further 2 hours
  5. customThe reaction product which had precipitated
  6. filtrationwas then filtered off
  7. washwashed with 100 ml of water
  8. customdried