HRID60131
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customobtained in (Example 3.15) <Step 2>
- distillationThereafter, about half of the solvent was distilled away under reduced pressure
- additionthe residue was then adjusted to pH 4 by addition of 3 N hydrochloric acid (50 ml)
- filtrationThe precipitated solid was collected by filtration
- washwas then successively washed with water (50 ml) and methyl tert-butyl ether (20 ml)