HRID874413

反应详情

EQUATION

反应方程式

HRID 874413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1 N sodium hydroxide aqueous solution (150 ml) was added to a methanol (150 ml) suspension of the methyl 2-bromo-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylate (10 g) obtained in (Example 3.15) <Step 2>, and the obtained mixture was then stirred for 30 minutes. Thereafter, about half of the solvent was distilled away under reduced pressure, and the residue was then adjusted to pH 4 by addition of 3 N hydrochloric acid (50 ml). The precipitated solid was collected by filtration, and was then successively washed with water (50 ml) and methyl tert-butyl ether (20 ml). The obtained solid was subjected to azeotropy with toluene to obtain the title compound (9.0 g) in the form of a white solid.

WORKUP

后处理

  1. customobtained in (Example 3.15) <Step 2>
  2. distillationThereafter, about half of the solvent was distilled away under reduced pressure
  3. additionthe residue was then adjusted to pH 4 by addition of 3 N hydrochloric acid (50 ml)
  4. filtrationThe precipitated solid was collected by filtration
  5. washwas then successively washed with water (50 ml) and methyl tert-butyl ether (20 ml)