HRID2061413

反应详情

EQUATION

反应方程式

HRID 2061413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(3,5-dibromo-4-hydroxyphenyl)ethanone (5.0 g, 17.01 mmol) and glyoxylic acid monohydrate (1.566 g, 17.01 mmol) in acetic acid (10 mL) was stirred and heated at reflux for 5 days. After this time, the precipitate formed was collected and recrystallised from toluene. This gave the title compound as a brown solid (4.674 g, 78%). 1H NMR δ (ppm) (DMSO-d6): 6.70 (1 H, d, J=15.45 Hz), 7.93 (1 H, d, J=15.46 Hz), 8.24 (2 H, s).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 5 days
  3. customAfter this time, the precipitate formed
  4. customwas collected
  5. customrecrystallised from toluene