HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → N-[4-(6,11-Dihydropyrido[2,3-b][1,5]benzodiazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepine | HCID 11030760 | — |
| Edukt | 4-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride | HCID 22099600 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-[4-(6,11-Dihydropyrido[2,3-b][1,5]benzodiazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide | HCID 22099880 | 30,2% |
Reaktionsschritte
A mixture of 0.197 g of 6,11-dihydropyrido[2,3-b][1,5]benzodiazepine, 0.444 g of 4-[([1,1'-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride and 0.155 g of N,N-diisopropylethylamine in 8 ml of dichloromethane is stirred at room temperature for 1.5 hours. The mixture is poured into water and extracted with dichloromethane. The extract is washed with H2O, saturated NaHCO3, H2O, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filtrate concentrated to dryness. The residue is chromatographed on thick layer silica gel plates with hexane-ethyl acetate (1:2) to give 0.160 g of solid, m.p. 147° C.-165° C. Anal Found: C, 72.1; H, 5.1; N, 9.1; Cl, 6.3.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05849735 |
| Quelldatensatz | uspto-grants-1998_12 |
| ORD ID | ord-8c6d6099666b4beb8d7db81577d9608d |
| Quellennotiz | uspto-grants-1998_12 |