HRID1095452

反应详情

EQUATION

反应方程式

HRID 1095452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5 mol % p-toluenesulphonic acid are added to a solution of 1 mmol of 5-hydroxy-5-(3H-imidazol-4-yl)-5,6,7,8-tetrahydronaphthalene-2-carbonitrile and 2.2 mmol of 2-mercaptoethanol [60-24-2] in 10 ml of xylene, and the mixture is heated to reflux in the presence of molecular sieves (4 Å) overnight. The reaction mixture is cooled to room temperature, diluted with 1M sodium bicarbonate solution and extracted with ethyl acetate (3×). The combined organic phases are dried with sodium sulphate and evaporated. The title compound is identified from the residue on the basis of the Rf by flash chromatography (SiO2 60F).

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureto reflux in the presence of molecular sieves (4 Å) overnight
  3. extractionextracted with ethyl acetate (3×)
  4. dry with materialThe combined organic phases are dried with sodium sulphate
  5. customevaporated