HRID2286485

反应详情

EQUATION

反应方程式

HRID 2286485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a four necked flask was charged 1.0 g of 1,3-dimethyl-4-(2,4-dichlorobenzoyl)-5-hydroxypyrazole, and the contents were dissolved in 20 ml of methyl ethyl ketone. 0.54 g of anhydrous potassium carbonate was added thereto, and 0.75 g of 1,1-dimethyl-2-chloroethyl bromomethyl ketone was further dropwise added while stirring whereby the mixture was reacted for 2 hours under the reflux condition (80° C.). After completion of the reaction, the reaction product was collected by filtration, and the solvent (methyl ethyl ketone) was distilled off to obtain a crude product. The crude product was passed through a silica gel column (eluent: methylene chloride), and the eluent was distilled off to obtain 0.7 g of the titled compound having a melting point of 58° to 60° C.

WORKUP

后处理

  1. customwas reacted for 2 hours under the reflux condition (80° C.)
  2. customAfter completion of the reaction
  3. filtrationthe reaction product was collected by filtration
  4. distillationthe solvent (methyl ethyl ketone) was distilled off
  5. customto obtain a crude product
  6. distillationthe eluent was distilled off