HRID725296

反应详情

EQUATION

反应方程式

HRID 725296 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.7 g of hydroxylamine, O-sulfonic acid in 6 ml of water is added to a solution of 1.83 g of 3,4-dihydroxy-5-nitrobenzaldehyde in 25 ml of water, subsequently stirred at 65° for 3.5 hours, cooled, the separated precipitate is filtered off under suction and taken up in ethyl acetate. The organic phase is dried over sodium sulfate and evaporated in a water-jet vacuum. The crystals obtained are recrystallized from ethyl acetate/n-hexane. There is obtained 3,4-dihydroxy-5-nitrobenzonitrile in the form of yellow crystals of m.p. 194°-195°.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationthe separated precipitate is filtered off under suction
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customevaporated in a water-jet vacuum
  5. customThe crystals obtained
  6. customare recrystallized from ethyl acetate/n-hexane