HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → HCID 44212555, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3-Cyclohexene-1-carbonyl chloride | HCID 523058 | — |
| Edukt | 5-(4-Aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine | HCID 15410467 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 44212555 | HCID 44212555 | 67,1% |
Reaktionsschritte
A mixture of 208 mg of 3-cyclohexene-1-carbonyl chloride (prepared from 3-cyclohexene-1-carboxylic acid and thionyl chloride) and 145 mg of triethylamine in 3 ml of methylene chloride is added to a solution of 377 mg of 5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine in 7 ml of methylene chloride. The mixture is stirred for 18 hours, washed with water, 1N HCl, water, 1M NaHCO3 and brine then dried with Na2 SO4. The organic layer is passed through a short column of hydrous magnesium silicate and hexane added to the filtrate at the boil to give 340 mg of the desired product as a crystalline solid, m.p. 234°-236° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05834461 |
| Quelldatensatz | uspto-grants-1998_11 |
| ORD ID | ord-144d35b463604f17845f918d3f2334ea |
| Quellennotiz | uspto-grants-1998_11 |