HRID1704471

反应详情

EQUATION

反应方程式

HRID 1704471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 52.5 parts of 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one hydrate in 200 parts of pyridine is added dropwise 63 parts of methanesulfonyl chloride. The mixture is stirred and cooled on the air for 2 hours. The pyridine is evaporated. To the residue is added 500 parts of water and the formed precipitate is filtered off. It is dissolved in 350 parts of trichloromethane. This solution is dried over magnesium sulfate and evaporated. The residue is crystallized from 40 parts of methylbenzene, yielding 25.5 parts of 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one methanesulfonate; mp. 118°-120° C.

WORKUP

后处理

  1. temperaturecooled on the air for 2 hours
  2. customThe pyridine is evaporated
  3. additionTo the residue is added 500 parts of water
  4. filtrationthe formed precipitate is filtered off
  5. dissolutionIt is dissolved in 350 parts of trichloromethane
  6. dry with materialThis solution is dried over magnesium sulfate
  7. customevaporated
  8. customThe residue is crystallized from 40 parts of methylbenzene