HRID236809

反应详情

EQUATION

反应方程式

HRID 236809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A portion of 4-bromophenol is converted to 4-bromo-2-nitrophenol by the method described in Rec. Trav. Chim. 29, 187(1910). A 28 g. portion of 4-bromo-2-nitrophenol is dissolved in 280 ml. of acetone. A 280 ml. portion of water and 112 g. of Na2S2O4 are added with stirring. The mixture is refluxed for 2 hours, cooled to room temperature and extracted six times with ether. The ether extracts are washed twice with brine, dried over magnesium sulfate and recrystallized from a mixture of charcoal and 400 ml. of water giving an oil. This oil is redissolved in 600 ml. of water, cooled to 0° C. and filtered giving 5-bromo-2-hydroxyaniline as tan crystals.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 2 hours
  2. extractionextracted six times with ether
  3. washThe ether extracts are washed twice with brine
  4. dry with materialdried over magnesium sulfate
  5. customrecrystallized from a mixture of charcoal and 400 ml
  6. dissolutionThis oil is redissolved in 600 ml
  7. temperatureof water, cooled to 0° C.
  8. filtrationfiltered