HRID1437285

反应详情

EQUATION

反应方程式

HRID 1437285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-(6-Methoxy-3-pyridazinyl)-5-(2-pyridyl)pyrazole-3-carboxylic acid methyl ester (2.20 g) obtained in Method B step 3) of Referential Example 139 was dissolved in a solvent mixture of methanol (30 mL) and tetrahydrofuran (30 mL), and 1N aqueous sodium hydroxide (15 mL) was added to the solution at room temperature, followed by stirring for 2.5 hours. Under cooling with ice, 1N aqueous hydrochloric acid (15 mL) and a solvent mixture of chloroform-methanol (10:1) were added to the reaction mixture for partitioning the mixture. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was removed under reduced pressure, and isopropyl ether was added to the residue, and then the precipitated solid was recovered by filtration, to thereby give the title compound (1.42 g, 47.6%).

WORKUP

后处理

  1. additionwas added to the solution at room temperature
  2. additionwere added to the reaction mixture
  3. customfor partitioning the mixture
  4. dry with materialThe organic layer was dried over sodium sulfate anhydrate
  5. filtrationfollowed by filtration
  6. customThe solvent was removed under reduced pressure, and isopropyl ether
  7. additionwas added to the residue
  8. filtrationthe precipitated solid was recovered by filtration