反应详情

A mixture of 5-(3-methylaminopropionyl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one (0.20 g) (J. Med. Chem., 1963, 6, 255), 4-methylphenethyl bromide (0.14 g) and sodium hydrogen carbonate (60 mg) in acetonitrile (20 ml) was heated under reflux for 16 hours and evaporated. The residue was partitioned between water and dichloromethane and the organic layer washed with brine, dried over MgSO4 and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-20% methanol as eluant. Appropriate fractions were combined and evaporated and the residue crystallised from ether to give the title compound as a colourless solid, 60 mg (21%).

1. temperaturewas heated
2. temperatureunder reflux for 16 hours
3. customevaporated
4. customThe residue was partitioned between water and dichloromethane
5. washthe organic layer washed with brine
6. dry with materialdried over MgSO4
7. customevaporated
8. customThe residue was purified by chromatography on silica
9. customevaporated
10. customthe residue crystallised from ether