HRID881982

反应详情

EQUATION

反应方程式

HRID 881982 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To solution of 1,3-dibromobenzene (84 g, 356 mmol) in DMF (700 ml) was added 1,2,3-1H-triazole (30 g, 427 mmol), Cul (6.8 g, 35.6 mmol), Iron(III) acetylacetonate (38 g, 107 mmol) and cesium carbonate (231 g, 712 mmol). The resulting mixture was heated to 120° C. under a nitrogen atmosphere overnight. After cooling to room temperature the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The obtained residue was purified using normal phase chromatography eluting with petroleum ether containing 20% ethyl acetate to give 2-(3-bromophenyl)-2H-1,2,3-triazole (28 g) and 1-(3-bromophenyl)-1H-1,2,3-triazole (11 g) as the pure isomers.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the reaction mixture
  2. filtrationwas filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe obtained residue was purified
  5. washeluting with petroleum ether containing 20% ethyl acetate