HRID53558
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 11-cyclopropyl-5,11-dihydro-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.5 g) and N-chlorosuccinimide (0.5 g) in carbon tetrachloride (50 mL) was heated under reflux for 6 hours. An additional 0.25 g of N-chlorosuccinimide was added and heating under reflux was continued for 4 hrs more. The mixture was filtered and the solvent was evaporated. The residue was fractionated over silica gel with ethyl acetate/hexane to give the title compound which crystallized from ethyl acetate/ethanol, m.p.>290° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 6 hours
- temperatureheating
- temperatureunder reflux
- filtrationThe mixture was filtered
- customthe solvent was evaporated