HRID2051686
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
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
- stirringstirring
- waitis continued for 3 hours
- temperatureat reflux temperature
- temperatureThe reaction mixture is cooled
- filtrationthe formed precipitate (sodium chloride) is filtered off
- customThe filtrate is evaporated
- customThe residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
- filtrationThe product is filtered off
- customdried