HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (4-Cyclohexyl-phenyl)-(4H,10H-3a,5,9-triaza-benzo[f]azulen-9-yl)-methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 16752034 | HCID 16752034 | — |
| Reactant | 4-Cyclohexylbenzoyl chloride | HCID 21890847 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | (4-Cyclohexyl-phenyl)-(4H,10H-3a,5,9-triaza-benzo[f]azulen-9-yl)-methanone | HCID 10156072 | 39.4% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07053083B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-804766a4845847baab408f4d922fc3cd |
| Source note | uspto-grants-2006_05 |