HRID59625

反应详情

EQUATION

反应方程式

HRID 59625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of ethyl-2-[(3-bromo-2-methoxyphenyl)hydrazono]-3-oxobutanoate (10 g) prepared as in Example 15, and 3,4-dimethylphenylhydrazine hydrochloride (6.05 g) and sodium acetate (2.63 g) in acetic acid (150 mL) was stirred and heated to about 80° C. to about 90° C. for about 3 hours. The reaction mixture was cooled to about room temperature and stirred for about 1 hour. The reaction mixture was filtered to give a solid, which was washed with acetic acid. The solid obtained was stirred in water for about 30 minutes at about room temperature, which was then filtered, washed with water and dried at about 55° C. to about 60° C. Yield: 11 g

WORKUP

后处理

  1. temperatureheated to about 80° C. to about 90° C. for about 3 hours
  2. temperatureThe reaction mixture was cooled to about room temperature
  3. stirringstirred for about 1 hour
  4. filtrationThe reaction mixture was filtered
  5. customto give a solid, which
  6. washwas washed with acetic acid
  7. customThe solid obtained
  8. filtrationwhich was then filtered
  9. washwashed with water
  10. customdried at about 55° C. to about 60° C