HRID2421533

反应详情

EQUATION

反应方程式

HRID 2421533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

2-Iodo-4-nitroaniline (5.3 g) in acetic acid (40 ml) was treated with 2,2,3 tribromopropanal (5.9 g) and the mixture was heated at 110° C. for 2 h after which it was cooled to room temperature and filtered. The filtered solid was washed with diethyl ether, suspended in water and treated with saturated sodium hydrogen carbonate. Extraction with ethyl acetate, drying over sodium sulphate, filtration and evaporation under reduced pressure gave the desired product, 3-bromo-8-iodo-6-nitro-quinoline, as a yellow solid after chromatography (silica; hexane/ethyl acetate) (M+379).

WORKUP

后处理

  1. temperaturewas cooled to room temperature
  2. filtrationfiltered
  3. washThe filtered solid was washed with diethyl ether
  4. additiontreated with saturated sodium hydrogen carbonate
  5. extractionExtraction with ethyl acetate
  6. dry with materialdrying over sodium sulphate, filtration and evaporation under reduced pressure