HRID274838

反应详情

EQUATION

反应方程式

HRID 274838 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a flask containing 1100 mL of water was added 97.20 grams (2.43 moles) of sodium hydroxide. When the sodium hydroxide was completely dissolved, 51.34 grams (0.162 mole) of 2,5-dichloro-3-iodobenzoic acid was added, turning the solution black. To this black solution was added 26.29 grams (0.105 mole) of copper(II) sulfate pentahydrate. The reaction mixture was heated to 100° C. and maintained at this temperature for three hours. At the-conclusion of this period, the reaction mixture was cooled in an icewater bath and then acidified with concentrated hydrochloric acid. This mixture was extracted with ethyl acetate, and the extract was washed four times with water and once with a saturated aqueous solution of sodium chloride. The extract was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated from the filtrate under reduced pressure, leaving 21.79 grams of 2,5-dichloro-3-hydroxybenzoic acid as a black solid.

WORKUP

后处理

  1. temperaturemaintained at this temperature for three hours
  2. waitAt the-conclusion of this period
  3. temperaturethe reaction mixture was cooled in an icewater bath
  4. extractionThis mixture was extracted with ethyl acetate
  5. washthe extract was washed four times with water
  6. dry with materialThe extract was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. customThe solvent was evaporated from the filtrate under reduced pressure