HRID231388

反应详情

EQUATION

反应方程式

HRID 231388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

(according to process A): ##STR19## 789 g (3.72 mols) of 4-amino-6-(1-cyclopropylethyl)-5-oxo-3-thioxo-tetrahydro-1,2,4-(2H,4H)-triazine are dissolved in a solution of 151 g (3.77 mols) of sodium hydroxide in 4 l of water. 3 ml of alkylarylpolyglycol ether are added, the mixture is cooled to 10° C., 542 g (3.82 mols) of methyl iodide are added and the mixture is stirred for 4 hours at room temperature. The mixture is filtered off with suction and the residue is washed with water and also with petroleum ether and dried at 60° C. in vacuo, after which 748 g (89% of theory) of the above compound of melting point 111°-113° C. are obtained. The purity as determined by gas chromatography is 99%.

WORKUP

后处理

  1. filtrationThe mixture is filtered off with suction
  2. washthe residue is washed with water and also with petroleum ether
  3. customdried at 60° C. in vacuo
  4. customafter which 748 g (89% of theory) of the above compound of melting point 111°-113° C. are obtained