HRID1065104
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- dissolutionWhen all of the product had dissolved
- customdid not exceed 30° C
- additionWhen the addition
- stirringthe reaction mixture was stirred at room temperature for a further 2 hours
- customThe reaction product which had precipitated
- filtrationwas then filtered off
- washwashed with 100 ml of water
- customdried