HRID1946448

反应详情

EQUATION

反应方程式

HRID 1946448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

4,5-Dihydro-6-isopropyl-3(2H)-pyridazinone (3.10 g) was dissolved in acetic acid (30.0 ml), and bromine (3.50 g, 22.0 mmol) was added dropwise to the solution over 10 minutes under heating at 100° C. with stirring. After the reaction solution was heated for 1 hour under reflux, the acetic acid was distilled away under reduced pressure, and water (100 ml) was added to the residues which were then extracted 5 times with ethyl acetate. The extracts were combined, dried over anhydrous magnesium sulfate and concentrated to give a crude product of 6-isopropyl-3(2H)-pyridazinone. The yield was 3.30 g.

WORKUP

后处理

  1. temperatureAfter the reaction solution was heated for 1 hour
  2. temperatureunder reflux
  3. distillationthe acetic acid was distilled away under reduced pressure, and water (100 ml)
  4. additionwas added to the residues which
  5. extractionwere then extracted 5 times with ethyl acetate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated