HRID1088331

反应详情

EQUATION

反应方程式

HRID 1088331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 11.3 parts of 4-(1H-imidazol-1-yl)benzenemethanol in 375 parts of trichloromethane was acidified with gaseous hydrogen chloride at room temperature. Then there were added dropwise 10.6 parts of thionyl chloride at room temperature. Upon completion, stirring was continued first for 30 minutes at reflux and further for 30 minutes at room temperature. The reaction mixture was evaporated. The residue was taken up a few times in methylbenzene and the latter was evaporated each time. The residue was stirred for 1 hour in 2,2'-oxybispropane. The product was filtered off, washed with 2,2'-oxybispropane and dried in vacuo overnight, yielding 13.5 parts of 1[4-(chloromethyl)phenyl]-1H-imidazole monohydrochloride (intermediate 20).

WORKUP

后处理

  1. customThe reaction mixture was evaporated
  2. customthe latter was evaporated each time
  3. stirringThe residue was stirred for 1 hour in 2,2'-oxybispropane
  4. filtrationThe product was filtered off
  5. washwashed with 2,2'-oxybispropane
  6. customdried in vacuo overnight