HRID9104

反应详情

EQUATION

反应方程式

HRID 9104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

General procedure for synthesizing 1-ethyl-5-methyl-3-(6-nitro-1,3-benzothiazol-2-yl)-1,3,5-triazinan-2-one: N-Ethyl-N′-(6-nitro-1,3-benzothiazol-2-yl)urea is suspended in an alkanol/water mixture, preferably 1:1 EtOH/H2O at room temperature. A 37% aqueous solution of formaldehyde is added followed by addition of a 2M solution of MeNH2 in MeOH, then about 2 mole equivalents of N-methylmorpholine. The solution is warmed to about 70–85° C., preferably 80° C., then allowed to stir for about 4–24 hours, preferably 4 hours. The slurry is then cooled to room temperature, filtered and washed well with water, dried and the title product is isolated. General Procedure for Grignard Addition:

WORKUP

后处理

  1. temperatureThe slurry is then cooled to room temperature
  2. filtrationfiltered
  3. washwashed well with water
  4. customdried