HRID2417914

反应详情

EQUATION

反应方程式

HRID 2417914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a stirred and cooled (0° C.) solution of 27.2 parts of 3-[(5-nitro-2-benzothiazolyl)amino]-1-propanol in 135 parts of N,N-dimethylformamide is added dropwise a solution of 15.7 parts of thionyl chloride in 45 parts of N,N-dimethylformamide. Upon completion, the whole is heated slowly to 120° C. and stirring at 120° C. is continued for 4 hours. The reaction mixture is cooled and the precipitated product is filtered off. It is washed with N,N-dimethylformamide and 2,2'-oxybispropane, and dried, yielding 24.4 parts (80%) of 3,4-dihydro-7-nitro-2H-pyrimido[2,1-b]benzothiazole monohydrochloride; mp. 328°-339° C.

WORKUP

后处理

  1. stirringstirring at 120° C.
  2. temperatureThe reaction mixture is cooled
  3. filtrationthe precipitated product is filtered off
  4. washIt is washed with N,N-dimethylformamide and 2,2'-oxybispropane
  5. customdried