HRID1630661

反应详情

EQUATION

反应方程式

HRID 1630661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.20 g (4.40 mmol) of ethyl 3-acetyl-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate were initially charged in in each case 30 ml of dioxane and methyl tert-butyl ether and 776 mg (4.85 mmol) of bromine were added dropwise at RT. The mixture was then stirred under reflux for 6 h. The reaction mixture was added to water, and the organic phase was separated off, dried over sodium sulphate and concentrated. The residue was recrystallized from methyl tert-butyl ether.

WORKUP

后处理

  1. additionwere added dropwise at RT
  2. temperatureunder reflux for 6 h
  3. customthe organic phase was separated off
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. customThe residue was recrystallized from methyl tert-butyl ether