HRID2254786

反应详情

EQUATION

反应方程式

HRID 2254786 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.0 g of ethyl (3,4-dihydroxy-5-nitrobenzoyl)acetate are suspended in 50 ml of ethanol. After treatment with 0.4 g of hydrazine hydrate the mixture is held at the reflux temperature for 16 hours. After distillation of the solvent, the residue is held at the boiling temperature for 5 minutes with 50 ml of ethyl acetate. The separated precipitate is filtered under suction and the filtrate is concentrated to 10 ml. The crystals, which separate in the cold, are filtered under suction. There is obtained 5-(5-hydroxypyrazol-3-yl)-3-nitropyrocatechol in form of orange crystals of m.p. 228° (dec.).

WORKUP

后处理

  1. distillationAfter distillation of the solvent
  2. filtrationThe separated precipitate is filtered under suction
  3. concentrationthe filtrate is concentrated to 10 ml
  4. customThe crystals, which separate in the cold,
  5. filtrationare filtered under suction