HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Dichlorobenzoyl chloride → HCID 67623947, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Dichlorobenzoyl chloride | HCID 78392 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-(4-Aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine | HCID 15410467 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 67623947 | HCID 67623947 | 76% |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
A mixture of 335 mg of 2,6-dichlorobenzoyl chloride and 258 mg of N,N-diisopropylethylamine is stirred in 2 ml of xylene while 314 mg of 5-(4-amino-benzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine is added. The reactants are refluxed in an oil bath at 110° C. for 18 hours. The xylene is evaporated in vacuo to a residue which is partitioned between methylene chloride and water. The organic layer is separated, washed with 1N HCl, 1 M NaHCO3, and brine. The organic layer is dried with Na2SO4 and passed through a pad of hydrous magnesium silicate. Hexane is added to the filtrate at the boil to give 370 mg of the desired product as a crystalline solid, m.p. 257°-259 ° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05786353 |
| Source dataset | uspto-grants-1998_07 |
| ORD ID | ord-c28b20431f014a5fa8ddd7ccf25af8ab |
| Source note | uspto-grants-1998_07 |