HRID2295043

反应详情

EQUATION

反应方程式

HRID 2295043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-(1-tert-butoxycarbonyl-4-methyl-5-benzimidazolyl)-N'-2-aminoethylthiourea (2.89 g) and mercuric acetate (3.32 g) in methanol (200 mL)/chloroform (100 mL) is stirred at room temperature for 2 hours. The resulting black mixture is filtered on Celite and the filtrate rotary evaporated. The residue is purified by flash chromatography on a short pad of silica gel, eluting with 10% methanol/chloroform containing 1% ammonium hydroxide. The product-containing fractions are collected and rotary evaporated to afford 1-tert-butoxycarbonyl-4-methyl-5-(2-imidazolinylamino)benzimidazole as a white solid.

WORKUP

后处理

  1. filtrationThe resulting black mixture is filtered on Celite
  2. customThe residue is purified by flash chromatography on a short pad of silica gel
  3. washeluting with 10% methanol/chloroform containing 1% ammonium hydroxide
  4. customThe product-containing fractions are collected
  5. customrotary evaporated