HRID2421525

反应详情

EQUATION

反应方程式

HRID 2421525 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 a stirred mixture of 3-bromo-6-hydroxyquinoline (preparation described in Liebigs Ann Chem (1966), 98-106) (1.0 g), sodium iodide (1.34 g) and copper iodide (0.09 g) in dioxane (6.5 ml) was added N,N,N′,N′-tetramethyl-ethane-1,2-diamine (0.1 ml) in a sealed tube. The mixture was stirred at 120° C. for 12 h and upon cooling was treated with aqueous ammonia followed by aqueous hydrochloric acid. Extraction with ethyl acetate, drying of the organic phase over magnesium sulphate, filtration and evaporation under reduced pressure gave the required product (MH+ 272) as a light brown coloured powder that was used as such in the next step.

WORKUP

后处理

  1. temperatureupon cooling
  2. extractionExtraction with ethyl acetate
  3. dry with materialdrying of the organic phase over magnesium sulphate, filtration and evaporation under reduced pressure