HRID248596

反应详情

EQUATION

反应方程式

HRID 248596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a 300 ml four-necked flask equipped with a stirrer, a thermometer and a condenser were charged 24.9 g (0.110 mol) of 1-bromo-2,5-dichlorobenzene, 13.19 g (0.143 mol) of thioglycolic acid, 12.06 g (0.286 mol) of 95% sodium hydroxide and 100 g of dimethylsulfoxide, followed by stirring at 120° C. for 4 hours. Then, after distilling off the dimethylsulfoxide under reduced pressure, 100 g of water was added to the residue. After dissolving the residue therein at 100° C., the solution was cooled for crystallization and filtered to yield sodium 2,5-dichlorophenylthioglycolate, which was then dissolved in 100 g of water with heating and acidized with concentrated hydrochloric acid, filtered and dried to yield 19.6 g of a light yellowish white powder of 2,5-dichlorophenylthioglycolic acid. The yield based on 1-bromo-2,5-dichlorobenzene was 75.1%.

WORKUP

后处理

  1. customTo a 300 ml four-necked flask equipped with a stirrer
  2. distillationThen, after distilling off the dimethylsulfoxide under reduced pressure, 100 g of water
  3. additionwas added to the residue
  4. dissolutionAfter dissolving the residue
  5. temperatureat 100° C., the solution was cooled for crystallization
  6. filtrationfiltered