HRID462224

反应详情

EQUATION

反应方程式

HRID 462224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture consisting of 3.8 gm., 0.0l55 mole of 2-(2-chloro- 5-thiadiazolyl)-1-methyl-5-nitroimidazole, prepared as in Example 16 2.5 gm., 0.029 mole of 3-dimethylaminopropylamine, 2.1 gm. 0.025 mole, of sodium bicarbonate and 100 ml. of benzene is refluxed for twenty-two hours. The reaction mixture is cooled to room temperature, washed with aqueous sodium bicarbonate and sodium chloride solutions. Cooling to 5° C. gives a crystalline precipitate which is collected and recrystallized from benzene to give the pure compound melting at 153°-154° C. More product is obtained from the mother liquors to give an overall yield of 3.0 gm.

WORKUP

后处理

  1. washwashed with aqueous sodium bicarbonate and sodium chloride solutions
  2. temperatureCooling to 5° C.
  3. customgives a crystalline precipitate which
  4. customis collected
  5. customrecrystallized from benzene