HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → (4-Cyclohexyl-phenyl)-(4H,10H-3a,5,9-triaza-benzo[f]azulen-9-yl)-methanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | HCID 16752034 | HCID 16752034 | — |
| Edukt | 4-Cyclohexylbenzoyl chloride | HCID 21890847 | — |
| Lösungsmittel | 1,2-Dichloroethane | HCID 11 | — |
| Produkt | (4-Cyclohexyl-phenyl)-(4H,10H-3a,5,9-triaza-benzo[f]azulen-9-yl)-methanone | HCID 10156072 | 39,4% |
Reaktionsschritte
A mixture of the 9,10-dihydro-4H-3a,5,9-triaza-benzo[f]azulene of Step D (4.67 mmol), 4-cyclohexylbenzoyl chloride (4.90 mmol) and triethylamine (5.1 mmol) in 1,2-dichloroethane was refluxed for three days under nitrogen. The solvent was removed in vacuo and the residue chromatographed on silica gel eluting with a solvent gradient from 5 to 20% of ethyl acetate in hexane to provide the title compound as a tan solid (0.684 g), m.p. 150-152° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07329653B2 |
| Quelldatensatz | uspto-grants-2008_02 |
| ORD ID | ord-217379c2778a40dc8199196fbaff8abc |
| Quellennotiz | uspto-grants-2008_02 |