HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,4-Dichlorobenzoyl chloride → Ethyl10-[4-[(2,4-dichlorobenzoyl)amino]-3-methylbenzoyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | ethyl 10,11-di-hydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate | HCID 21836996 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Ethyl10-[4-[(2,4-dichlorobenzoyl)amino]-3-methylbenzoyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate | HCID 21837013 | 55,4% |
Reaktionsschritte
To a solution of 0.30 g of ethyl 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate in 20 ml of methylene chloride is added 0.15 g of N,N-diisopropylethylamine and 0.24 g of 2,4-dichlorobenzoyl chloride. The reaction mixture is stirred at room temperature for 18 hours and washed with water, saturated NaHCO3 and dried with Na2SO4. The organic layer is passed through a pad of hydrous magnesium silicate. Hexane is added to the filtrate at the boil to give 0.24 g of solid, m.p. 174°-184° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05624923 |
| Quelldatensatz | uspto-grants-1997_04 |
| ORD ID | ord-7a67b3d438a44186b206d8ecf36fbdb0 |
| Quellennotiz | uspto-grants-1997_04 |