HRID2051686

反应详情

EQUATION

反应方程式

HRID 2051686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 25 parts of 1,3-dihydro-1-methyl-2H-benzimidazol-2-one, 64 parts of sodium methanolate solution 30% and 240 parts of methanol is stirred for one hour at room temperature. Then there are added 27.88 parts of 3-(chloromethyl)pyridine hydrochloride and stirring is continued for 3 hours at reflux temperature. The reaction mixture is cooled and the formed precipitate (sodium chloride) is filtered off. The filtrate is evaporated. The residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane. The product is filtered off and dried, yielding 16 parts (39.3%) of 1,3-dihydro-1-methyl-3-(3-pyridinylmethyl)-2H-benzimidazol-2-one; mp. 90° C.

WORKUP

后处理

  1. stirringstirring
  2. waitis continued for 3 hours
  3. temperatureat reflux temperature
  4. temperatureThe reaction mixture is cooled
  5. filtrationthe formed precipitate (sodium chloride) is filtered off
  6. customThe filtrate is evaporated
  7. customThe residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
  8. filtrationThe product is filtered off
  9. customdried