HRID1750232

反应详情

EQUATION

反应方程式

HRID 1750232 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.26 g 4-((1R,2R)-2-Methyl-cyclohexylamino)-3-(2-thiazol-5-yl-acetylamino)-benzoic acid methyl ester in 10 ml dioxane were added 12 ml of 4M hydrochloric acid in dioxane and the mixture was heated to reflux for 2 h. The reaction was concentrated and the residue was taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution and brine. The organic layers were dried over sodium sulphate and concentrated. The resulting residue was purified by HPLC to yield 0.37 g (31%) of 1-((1R,2R)-2-Methyl-cyclohexyl)-2-thiazol-5-ylmethyl-1H-benzoimidazole-5-carboxylic acid methyl ester.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 2 h
  3. concentrationThe reaction was concentrated
  4. washwashed with saturated aqueous sodium bicarbonate solution and brine
  5. dry with materialThe organic layers were dried over sodium sulphate
  6. concentrationconcentrated
  7. customThe resulting residue was purified by HPLC