HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22099630, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepine | HCID 11030760 | — |
| Reactant | 4-(2-Phenylbenzoylamino)-benzoylchloride | HCID 11450501 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22099630 | HCID 22099630 | — |
Reaction Steps
A mixture of 0.296 g of 6,11-dihydropyrido[2,3-b][1,5]benzodiazepine, 0.604 g of 4-[([1,1'-biphenyl]-2-carbonyl)amino]benzoyl chloride and 0.232 g of N,N-diisopropylethylamine in 6 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 purified on thick layer silica gel plates with hexane-ethyl acetate (1:2) as solvent to give the product as a solid which is crystallized from ethyl acetate to give off-white crystals, m.p. 220° C.-221° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05849735 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-b2719f5e9e164323ab503520af800101 |
| Source note | uspto-grants-1998_12 |