HRID896318

反应详情

EQUATION

反应方程式

HRID 896318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(2-Oxo-2,3-dihydro-benzoimidazol-1-yl)-acetic acid tert-butyl Ester (399 mg, 1.61 mmol) in CH2Cl2 (15 ml) was trreated with BTPP and then treated with 2-chloromethyl-1-(3-methyl-butyl)-1H-benzoimidazole-5-carbonitrile (400 mg, 1.53 mmol). The reaction was stirred for 25 min then the mixture was diluted with ether and washed with water. The organic layer was dried over MgSO4, concentrated and the residue purified by column chromatography with gradient elution using first 1:1 EtOAc in hexanes then 2:1 EtOAc in hexanes to give 1.52 g (99%) of {3-[5-Cyano-1-(3-methyl-butyl)-1H-benzoimidazol-2-ylmethyl]-2-oxo-2,3-dihydro-benzoimidazol-1-yl}-acetic acid tert-butyl ester as a white solid.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over MgSO4
  3. concentrationconcentrated
  4. customthe residue purified by column chromatography with gradient elution