HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Bicarbonate → 5-{3-[N-(4-Methylphenethyl)-N-methylamino]propionyl}-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 4-Methylphenethyl bromide | HCID 570680 | — |
| Edukt | 5,10-Dihydro-5-[3-(methylamino)-1-oxopropyl]-11H-dibenzo[b,e][1,4]diazepin-11-one | HCID 20802897 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 5-{3-[N-(4-Methylphenethyl)-N-methylamino]propionyl}-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one | HCID 53993990 | — |
Reaktionsschritte
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%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05418229 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-f317d4907b7246d2bd8a17afb1447994 |
| Quellennotiz | uspto-grants-1995_05 |