HRID59619

反应详情

EQUATION

反应方程式

HRID 59619 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-(3,4-dimethylphenyl)-3-methyl-4-(3-bromo-2-methoxyphenyl)hydrazono-5-pyrazolone(5 g) prepared as in Example 2, in 48% aqueous hydrobromic acid (200 mL) and glacial acetic acid (50 mL) was stirred and heated under reflux for about 80 hours. The reaction mixture was concentrated under vacuum to obtain a thick residue. Water (40 mL) was added and basified to pH 7-8 using saturated solution of sodium bicarbonate (20 mL). The mixture was filtered to give an orange solid, which was washed with water (25 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours. Yield: 3.5 g

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for about 80 hours
  3. concentrationThe reaction mixture was concentrated under vacuum
  4. customto obtain a thick residue
  5. filtrationThe mixture was filtered
  6. customto give an orange solid, which
  7. washwas washed with water (25 mL)
  8. customdried in an oven at about 55° C. to about 60° C. for about 12 hours