HRID2267173

反应详情

EQUATION

反应方程式

HRID 2267173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4N Hydrochloric acid solution in dioxane (10 ml) was added to 3 mg of tert-Butyl 4-[1-(2-chloropyridin-3-yl)-5-methyl-1H-[1,2,3]triazol-4-yl)-piperazine-1-carboxylate prepared in Example 34, the mixture was stirred at room temperature for 3 hours, the solvent was evaporated in vacuo, the residue was dissolved in 1 ml of chloroform and, in a nitrogen atmosphere, 0.03 ml of isopropyl chloroformate and 0.06 ml of triethylamine were added thereto and the mixture was stirred at room temperature for 2 hours. After the solvent was evaporated in vacuo, the resulting residue was purified by a preparative thin-layer silica gel chromatography (chloroform:methanol=9:1) to give 2 mg of the title compound as a white solid.

WORKUP

后处理

  1. customthe solvent was evaporated in vacuo
  2. dissolutionthe residue was dissolved in 1 ml of chloroform and, in a nitrogen atmosphere, 0.03 ml of isopropyl chloroformate and 0.06 ml of triethylamine
  3. additionwere added
  4. stirringthe mixture was stirred at room temperature for 2 hours
  5. customAfter the solvent was evaporated in vacuo
  6. customthe resulting residue was purified by a preparative thin-layer silica gel chromatography (chloroform:methanol=9:1)