HRID1638395

反应详情

EQUATION

反应方程式

HRID 1638395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-[bis(isodecyloxycarbonyl)methyl]-1,2,4-triazole (51.8 g, 86% strength) was stirred and boiled under reflux at 78° with carbon tetrachloride (100 cm3) whilst bromine (16.0g) was added slowly beneath the liquid surface during 30 minutes. Stirring and heating at 78°-80° was continued for a further period of 2 hours, the extent of bromination being followed by disappearance of the resonance due to the methine proton at delta=5.8 ppm from tetramethylsilane in the nmr spectrum. The solution was then cooled, washed with dilute aqueous sodium sulphite solution and with water, and the solvent was distilled yielding 57.2 g of 1-[1',1'-bis(isodecyloxycarbonyl)-1'-bromomethyl]-1,2,4-triazole of strength 76% as measured by non-aqueous titration with perchloric acid. This compound was evaluated as an extractant for copper using the procedure of Example 1 and the results are presented in Table 1.

WORKUP

后处理

  1. additionwas added slowly beneath the liquid surface during 30 minutes
  2. temperatureheating at 78°-80°
  3. temperatureThe solution was then cooled
  4. washwashed with dilute aqueous sodium sulphite solution and with water
  5. distillationthe solvent was distilled