HRID46879
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 5 parts of 1,3-dihydro-1-(3-iodopropyl)-3-methyl-2H-benzimidazol-2-one, 3.75 parts of 5-chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 2,65 parts of sodium carbonate and 22.5 parts of N,N-dimethylformamide is stirred at 70°-80° C. for 2 hours. The reaction mixture is cooled, poured onto water and the precipitated product is filtered off. It is dissolved in trichloromethane. The solution is dried, filtered and evaporated. The residue is crystallized from 4-methyl-2-pentanone, yielding 3 parts (43%) of 5-chloro-1-{1-[3-(1,3-dihydro-3-methyl-2-oxo-2H-benzimidazol-1-yl)propyl]-4-piperidinyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 166.5° C.
WORKUP
后处理
- temperatureThe reaction mixture is cooled
- additionpoured onto water
- filtrationthe precipitated product is filtered off
- dissolutionIt is dissolved in trichloromethane
- customThe solution is dried
- filtrationfiltered
- customevaporated
- customThe residue is crystallized from 4-methyl-2-pentanone