HRID258834

反应详情

EQUATION

反应方程式

HRID 258834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 26 parts of 1,3-dihydro-1-(2-hydroxyethyl)-5-methyl-2H-benzimidazol-2-one and 390 parts of trichloromethane are added dropwise 48 parts of sulfinyl chloride at room temperature. Upon completion, stirring is continued for 5 hours at reflux. The reaction mixture is evaporated. The oily residue is heated with 2,2'-oxybispropane and a small amount of 2-propanol and the whole is stirred with activated charcoal. The latter is filtered off and the filtrate is stirred at room temperature till all the product is precipitated. It is filtered off and dried, yielding 12 parts (42%) of 1-(2-chloroethyl)-1,3-dihydro-5-methyl-2H-benzimidazol-2-one; mp. 120° C.

WORKUP

后处理

  1. temperatureat reflux
  2. customThe reaction mixture is evaporated
  3. temperatureThe oily residue is heated with 2,2'-oxybispropane
  4. stirringa small amount of 2-propanol and the whole is stirred with activated charcoal
  5. filtrationThe latter is filtered off
  6. stirringthe filtrate is stirred at room temperature till all the product
  7. customis precipitated
  8. filtrationIt is filtered off
  9. customdried