HRID1436705
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
Treat a solution of 5-(1-hydroxyethyl)-N-methyl-N-propyl-isophthalamic acid ethyl ester (250 mg, 0.85 mmol) in dichloromethane (10 mL) with Dess-Martin periodinane (470 mg, 1.11 mmol). Stir at room temperature for 2.5 h, quench with 10% aqueous sodium sulfate, extract with ethyl acetate (50 mL). Wash with 10% aqueous sodium sulfate solution, saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes) to give the title compound (196 mg, 78%).
WORKUP
后处理
- customquench with 10% aqueous sodium sulfate
- extractionextract with ethyl acetate (50 mL)
- washWash with 10% aqueous sodium sulfate solution, saturated aqueous sodium chloride
- dry with materialdry (magnesium sulfate)
- concentrationconcentrate
- custompurify
- wash(silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes)