HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → N-[4-[(5,11-Dihydro-10H-dibenz[b,e][1,4]diazepin-10-yl)carbonyl]-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 10,11-Dihydro-5h-dibenzo[b,e][1,4]diazepine | HCID 36046 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 4-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride | HCID 22099600 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-[4-[(5,11-Dihydro-10H-dibenz[b,e][1,4]diazepin-10-yl)carbonyl]-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide | HCID 22099587 | 58,6% |
Reaktionsschritte
A mixture of 0.196 g of 5,11-dihydro-10H-dibenzo[b,e][1,4]diazepine, 0.155 g of N,N-diisopropylethylamine and 0.444 g of 4-[([1,1'-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride in 12 ml of dichloromethane is stirred at room temperature overnight. The mixture is poured into water and extracted with dichloromethane. The extract is washed with 2N K2CO3, H2O, brine and dried (Na2 SO4). The solution is filtered through a thin pad of hydrous magnesium silicate. The filtrate is concentrated to dryness and the residue triturated with ether and the solvent removed. The residue is triturated with dichloromethane to give 0.31 g of solid, m.p. 158° C.-184° C. Anal. Found for C33H24ClN3O2 1/2 H2O; C,73.7; H, 4.6; N,7.5; Cl,6.9.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05849735 |
| Quelldatensatz | uspto-grants-1998_12 |
| ORD ID | ord-5bbc1f50d4854d4591f113cea24b666b |
| Quellennotiz | uspto-grants-1998_12 |