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-amino-benzoyl)-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, I N 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 | US05686445 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-b7ef9d3d216d488791af29245981592f |
| Source note | uspto-grants-1997_11 |