HRID1610586
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
To a solution of 5-phenoxypyridine-2-carboxylic acid (10 g, 46.5 mmol) in tetrahydrofuran (150 ml) was added N,N′-carbonyldiimidazole (8.29. g, 51.1 mmol), and the mixture was heated under reflux for 1 hr. After cooling the reaction solution to room temperature, monobenzyl malonate magnesium salt (10.5 g, 25.6 mmol) was added, and the mixture was heated under reflux for 2 hrs. The reaction solution was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1) to give the objective substance (11.2 g, 76%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 1 hr
- temperaturethe mixture was heated
- temperatureunder reflux for 2 hrs
- concentrationThe reaction solution was concentrated
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1)
- customto give the objective substance (11.2 g, 76%)