HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Methylpiperazine → 1,3-Dimethyl-4-[3-(4-methyl-1-piperazinyl)propionyl]-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Methylpiperazine | HCID 53167 | — |
| Edukt | 4-(3-Bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one | HCID 20515487 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 1,3-Dimethyl-4-[3-(4-methyl-1-piperazinyl)propionyl]-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one | HCID 20515446 | 76% |
Reaktionsschritte
1.5 g of 4-(3-bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one and 0.85 g of N-methylpiperazine are warmed at 80° C. for 15 hours in 50 ml of dioxane. The thus-obtained mixture is concentrated to dryness in vacuo. 20 ml of saturated aqueous sodium carbonate solution are added thereto with stirring, and the mixture is then extracted three times with ethyl acetate. The combined extracts are dried over sodium sulfate, and the solvent is stripped off in vacuo. The resulting residue is chromatographed on neutral silica gel (methylene chloride/methanol 95/05). 1.2 g of the title compound of m.p. 187° C. (from isopropanol) are obtained).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04363816 |
| Quelldatensatz | uspto-grants-1982_12 |
| ORD ID | ord-5438a24a039444bb838c30312aec8c6f |
| Quellennotiz | uspto-grants-1982_12 |