HRID1274393
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 suspension of pyridin-3-yl-acetic acid (856 mg in 20 mL dry methylene chloride) was added in sequence 0.35 mL triethylamine, 1-hydroxybenzotriazole (862 mg) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.08 g) and the reagents allowed to mix for 1 hour. At this time, N,O-dimethylhydroxylamine hydrochloride (1.22 g) was added followed by 2.0 mL triethylamine and the reaction stirred at room temperature. After 20 hours, the mixture applied to a silica gel column and purified by flash chromatography (methylene chloride:methanol, 94:6) to give the title compound (796 mg).
WORKUP
后处理
- additionto mix for 1 hour
- custompurified by flash chromatography (methylene chloride:methanol, 94:6)