HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67624719, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3,5-Dichlorobenzoyl chloride | HCID 76191 | — |
| Reactant | 5-(4-Aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine | HCID 15410467 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67624719 | HCID 67624719 | 49.7% |
Reaction Steps
A mixture of 301.6 mg of 3,5-dichlorobenzoyl chloride and 145 mg of triethylamine is stirred in 2 ml of methylene chloride while 314 mg of 5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine in 5 ml of methylene chloride is added. The reaction mixture is stirred at room temperature for 2 hours and 100 mg of 3,5-dichlorobenzoyl chloride added. The reactants are heated at reflux for 36 hours. The cooled reaction mixture layer washed with 1N HCl, water, 1N NaOH, water and brine. The organic layer is dried with Na2SO4 and passed through a short pad of hydrous magnesium silicate and hexane added to the filtrate at the boil to give 242 mg of the desired product as a crystalline solid, m.p. 263°-265° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05854236 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-108b3a176f004867b82ee8ae9325988e |
| Source note | uspto-grants-1998_12 |