HRID41858

反应详情

EQUATION

反应方程式

HRID 41858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 610 mg (1.34 mmol) of methyl 5-(3,5-bistrifluoromethylpyrazol-1-ylmethyl)-2-(3-chloropyridin-2-yl)-2H-pyrazole-3-carboxylate in 9 ml of ethanol is admixed dropwise with a solution of 699 mg (1.78 mmol) of sodium hydroxide in 7 ml of water. The mixture is stirred at room temperature for 2 hours and concentrated to about 5 ml on a rotary evaporator. This residue is admixed with 5 ml of tert-butyl methyl ether and the organic phase is subsequently washed with water. The combined aqueous phases are adjusted to a pH of about 3 with concentrated hydrochloric acid, with ice cooling, and are extracted with three times 50 ml of ethyl acetate. The combined organic phases are dried over magnesium sulphate and then the solvent is removed on a rotary evaporator.

WORKUP

后处理

  1. concentrationconcentrated to about 5 ml on a rotary evaporator
  2. washthe organic phase is subsequently washed with water
  3. extractionare extracted with three times 50 ml of ethyl acetate
  4. dry with materialThe combined organic phases are dried over magnesium sulphate
  5. customthe solvent is removed on a rotary evaporator