HRID252614

反应详情

EQUATION

反应方程式

HRID 252614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 0.56 g (0.8 mmol) ethyl-4-(1-hydroxy-1-methylethyl)-2-propyl-1-[(2′-cyanobiphenyl-4-yl)-methyl]-imidazole-5-carboxylate, 3 ml toluene, 0.65 ml (2.1 mmol) tributyltin chloride and 0.13 mg (2 mmol) NaN3, were heated under reflux for 42 h. The reaction mixture was evaporated under reduced pressure and the residue was dissolved in 5.5 ml of 2.5 M HCl in ethanol. The solution was stirred for 18 h and then concentrated. The residue was triturated in diisopropyl ether to give 0.51 g of the title compound as hydrochloride salt.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureunder reflux for 42 h
  3. customThe reaction mixture was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in 5.5 ml of 2.5 M HCl in ethanol
  5. concentrationconcentrated
  6. customThe residue was triturated in diisopropyl ether