HRID732417
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Add a suspension of potassium peroxymonosulfate (35.6 g, 57.7 mmol) in water (80 mL) to a cooled solution of 2-chloro-6-propylsulfanyl-isonicotinic acid methyl ester (4.71 g, 19.2 mmol) in methanol (40 mL) and THF (40 mL). Stir the mixture at room temperature for 3 days. Dilute the mixture with water and extract with dichloromethane (3×100 mL). Wash the combined extracts with water, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 20:80 ethyl acetate:hexanes) to give the title product (2.75 g, 52%).
WORKUP
后处理
- additionAdd
- extractionextract with dichloromethane (3×100 mL)
- washWash the combined extracts with water
- dry with materialdry (magnesium sulfate)
- concentrationconcentrate
- custompurify
- wash(silica gel chromatography, eluting with 20:80 ethyl acetate:hexanes)