HRID2417914
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
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
- stirringstirring at 120° C.
- temperatureThe reaction mixture is cooled
- filtrationthe precipitated product is filtered off
- washIt is washed with N,N-dimethylformamide and 2,2'-oxybispropane
- customdried