HRID1264621

反应详情

EQUATION

反应方程式

HRID 1264621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 4-hydroxy-3-nitrophenylacetate (21.1 g, 0.1 mol) was suspended in a mixture of water (55 ml) and methanol (105 ml). The suspension was stirred at room temperature while a solution of sodium hydroxide (8.8 g, 0.22 mol) in water (50 ml) was added dropwise over 20 minutes, maintaining the reaction temperature between 20 and 25° C. by water bath cooling. The resultant dark red solution was stirred at room temperature for 15 minutes, diluted with water and acidified to pH1-2 by addition of 2M hydrochloric acid and extracted with ethyl acetate. The organic extract was washed with brine (200 ml), dried over magnesium sulphate, filtered and concentrated under reduced pressure to give 4-hydroxy-3-nitrophenylacetic acid (19.6 g) as a yellow solid.

WORKUP

后处理

  1. additionwas added dropwise over 20 minutes
  2. temperaturemaintaining the reaction temperature between 20 and 25° C. by water bath
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. extractionThe organic extract
  6. washwas washed with brine (200 ml)
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure