HRID126872

反应详情

EQUATION

反应方程式

HRID 126872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.92 parts of 1-(2-chloroethyl)-1,3-dihydro-2H-benzimidazol-2-one, 5.4 parts of 1-(4-methoxyphenyl)-2-(4-piperidinyl)ethanone hydrochloride, 5.3 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is distilled azeotropically to dry overnight. After cooling, the precipitated product is filtered off, washed with water and dissolved in trichloromethane. The latter is dried, filtered and evaporated. The residue is crystallized from 2-propanol, yielding 2.9 parts (36.5%) of 1,3-dihydro-1-[2-[4-[2-(4-methoxyphenyl)-2-oxoethyl]-1-piperidinyl]ethyl]-2H-benzimidazol-2-one; mp. 155.9° C.

WORKUP

后处理

  1. distillationis distilled azeotropically
  2. customto dry overnight
  3. temperatureAfter cooling
  4. filtrationthe precipitated product is filtered off
  5. washwashed with water
  6. dissolutiondissolved in trichloromethane
  7. customThe latter is dried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue is crystallized from 2-propanol