تفاعل #65133

معادلة التفاعل

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

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةunder reflux for 16 hours
3. 3
   أخرىevaporated
4. 4
   أخرىThe residue was partitioned between 2M aqueous sodium hydrogen carbonate solution and dichloromethane
5. 5
   غسيلthe organic layer washed with brine
6. 6
   تجفيفdried over MgSO4
7. 7
   أخرىevaporated
8. 8
   أخرىThe residue was purified by chromatography on silica
9. 9
   أخرىevaporated
10. 10
    أخرىthe residue crystallised from ethyl acetate

الإجراء التجريبي

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%).

المصدر