HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| Edukt | 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide | HCID 20041714 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate | HCID 19833914 | — |
Reaktionsschritte
1.19 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide are dissolved in 10 ml of methylene chloride, and the solution is treated with 1.14 g of triethyloxonium tetrafluoroborate and stirred at room temperature for 20 hours. The mixture is then poured on to 10% sodium carbonate solution/ice and the whole is extracted with methylene chloride. The combined extracts are washed with 10% sodium carbonate solution, dried over anhydrous sodium sulphate and evaporated under reduced pressure. In this manner there is obtained crude ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-caboximidate which is purified by a filtration on silica gel [eluent: n-hexane/ethyl acetate (1:1)]; m.p. 74°-76° C. (crystallized from n-hexane).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04766115 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-62a3a9f5b00e4b3493aa4800d32f3db5 |
| Quellennotiz | uspto-grants-1988_08 |