HRID552910
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
27.50 g (91.3 mmol) of 4-[(3-chloropropyl)[(6-chloropyridin-3-yl)methyl]amino]furan-2(5H)-one (I-2) and 51.60 g (344.2 mmol) of sodium iodide in 1.2 l of acetonitrile are heated under reflux for 4 hours. Concentration of the organic phase under reduced pressure and purification of the residue by column chromatography on silica gel (silica gel 60, Merck, particle size: 0.04 to 0.063 mm) using the mobile phase ethyl acetate gives 31.5 g of 4-[[(6-chloropyridin-3-yl)methyl](3-iodopropyl)amino]furan-2(5H)-one.
WORKUP
后处理
- temperatureunder reflux for 4 hours
- customConcentration of the organic phase under reduced pressure and purification of the residue by column chromatography on silica gel (silica gel 60, Merck, particle size: 0.04 to 0.063 mm)