HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanol → 5,10-Dihydro-5-[3-pyrrolidino-propionyl]-11H-dibenzo[b,e][1,4]diazepin-11-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Acryloyl chloride | HCID 13140 | — |
| Edukt | Pyrrolidine | HCID 31268 | — |
| Edukt | 5,10-Dihydro-11H-dibenzo(b,e)(1,4)diazepin-11-one | HCID 201327 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 5,10-Dihydro-5-[3-pyrrolidino-propionyl]-11H-dibenzo[b,e][1,4]diazepin-11-one | HCID 12834683 | — |
Reaktionsschritte
6.3 gm (0.03 mol) of 5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one and 3.3 gm (0.036 mol) of acrylic acid chloride were refluxed, while stirring, in 200 ml of toluene for 3 hours. The reaction mixture was then evaporated in vacuo. The dry residue was admixed with 200 ml of ethanol, and 2.5 gm (0.035 mol) of pyrrolidine were added dropwise, while stirring, to the boiling solution. Subsequently, the reaction mixture was heated for 20 minutes, then evaporated in vacuo to about 1/10 of its original volume, and discolored by filtration through activated charcoal/silica gel. The crude product was recrystallized from a little ethyl acetate.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04377576 |
| Quelldatensatz | uspto-grants-1983_03 |
| ORD ID | ord-993854165d8f4ec4a76a748cfa519fad |
| Quellennotiz | uspto-grants-1983_03 |