HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,8-Diazabicyclo(5.4.0)undec-7-ene → 7-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Edukt | 8-Chloro-1-cyclopropyl-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid | HCID 9835941 | — |
| Edukt | tert-Butyl (4-methylpyrrolidin-3-yl)carbamate | HCID 14738853 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 7-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid | HCID 13933093 | 50% |
Reaktionsschritte
A mixture of 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.5 g), anhydrous acetonitrile (5 ml), 3-t-butoxycarbonylamino-4-methylpyrrolidine (0.5 g) and DBU (0.25 g) was refluxed for an hour. The reacting mixture was concentrated under reduced pressure, to the resulting residue was added acetonitrile-ether (1:1) to crystallize and the precipitate was collected by filtration. This precipitate was recrystallized from dichloromethane-methanol to give the title compound (0.4 g) as pale yellow powder, mp 213°-215° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04753953 |
| Quelldatensatz | uspto-grants-1988_06 |
| ORD ID | ord-93b09440a0084f409c18a4bd37004c23 |
| Quellennotiz | uspto-grants-1988_06 |