HRID70794

反应详情

EQUATION

反应方程式

HRID 70794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An aqueous solution (30 ml) of potassium cyanide (15 g) was ice-cooled, then, an EtOH (140 ml) solution of 2-(chloromethyl)-4,5,6,7-tetrahydro-1H-benzimidazole hydrochloride (12.0 g) was added, and stirring was performed at room temperature for 1 hour and then at 50° C. for 1, hour. A saturated aqueous sodium hydrogen carbonate solution was added to the reaction liquid, followed by concentration under reduced pressure and extraction with chloroform. The organic layer was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (28% aqueous ammonia/methanol/chloroform) to obtain 4,5,6,7-tetrahydro-1H-benzimidazol-2-yl acetonitrile (8.6 g).

WORKUP

后处理

  1. temperaturecooled
  2. customat 50° C.
  3. concentrationfollowed by concentration under reduced pressure and extraction with chloroform
  4. concentrationThe organic layer was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (28% aqueous ammonia/methanol/chloroform)