HRID53558

反应详情

EQUATION

反应方程式

HRID 53558 的结构方程式

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

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. temperatureheating
  4. temperatureunder reflux
  5. filtrationThe mixture was filtered
  6. customthe solvent was evaporated