HRID1110091

反应详情

EQUATION

反应方程式

HRID 1110091 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The bromination reaction takes place in carbon tetrachloride with N-bromosuccinimide and AIBN as radical former. For this purpose, an equimolar amount of ester (i) and 0.45 mole N-bromosuccinimide are mixed with 300 ml. carbon tetrachloride and a spatula tip of AIBN added thereto. The reaction mixture is heated under reflux for 4 hours, subsequently allowed to cool and the precipitated succinimide (0.41 mole; 92% of theory) is filtered off. After distilling off the solvent in a vacuum, the residue is purified by column chromatography using PE/EE (25:1 v/v) as elution agent. The end product obtained is a yellow oil. The yield of 75% of theory. C6H6O2BrCl3 (296.3752 g./mole).

WORKUP

后处理

  1. customThe bromination reaction
  2. temperatureThe reaction mixture is heated
  3. temperatureunder reflux for 4 hours
  4. temperatureto cool
  5. distillationAfter distilling off the solvent in a vacuum
  6. customthe residue is purified by column chromatography
  7. washas elution agent
  8. customThe end product obtained