反応 #65133

反応方程式

11-chloroacetyl-5,11-dihydro-6H-pyrido- [2,3-b][1,4]benzodiazepine-6-one

N-(4-methoxyphenethyl)methylamine

sodium hydrogen carbonate

acetonitrile

→

title compound

5,11-Dihydro-11-{2-[N-(4-methoxyphenethyl)-N-methylamino]acetyl}-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度under reflux for 16 hours
3. 3
   その他evaporated
4. 4
   その他The residue was partitioned between 2M aqueous sodium hydrogen carbonate solution and dichloromethane
5. 5
   洗浄the organic layer washed with brine
6. 6
   乾燥dried over MgSO4
7. 7
   その他evaporated
8. 8
   その他The residue was purified by chromatography on silica
9. 9
   その他evaporated
10. 10
    その他the residue crystallised from ethyl acetate

実験手順

A mixture of 11-chloroacetyl-5,11-dihydro-6H-pyrido- [2,3-b][1,4]benzodiazepine-6-one (288 mg) (German patent 1,936,670), N-(4-methoxyphenethyl)methylamine (182 mg) and sodium hydrogen carbonate (92 mg) in acetonitrile (25 ml) was heated under reflux for 16 hours and evaporated. The residue was partitioned between 2M aqueous sodium hydrogen carbonate solution 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 0-10% methanol as eluant. Appropriate fractions were combined and evaporated and the residue crystallised from ethyl acetate to give the title compound as a colourless solid, 216 mg (52%).

出典