Reaktionsgleichung
Cl[C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[C:4]#[N:5].[N:13]1(C(O)C)[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.[CH2:22]([OH:24])[CH3:23]>>[N+:10]([C:7]1[CH:8]=[CH:9][C:2]([N:13]2[CH2:14][CH2:15][NH:16][CH2:17][CH:18]2[CH2:23][CH2:22][OH:24])=[C:3]([CH:6]=1)[C:4]#[N:5])([O-:12])=[O:11]Komponenten
4
Versuchsvorschrift
2-Chloro-5-nitrobenzonitrile (15 g) and piperazinoethanol (16 g) were added to ethanol (100 ml) and the mixture was stirred at a refluxing temperature for 1 h. The solvent was evaporated under reduced pressure. To the residue was added aqueous sodium hydroxide solution and the mixture was extracted with chloroform. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, after which the solvent was evaporated under reduced pressure. To the residue diisopropyl ether was added to allow crystallization. The crystals were recrystallized from hydrous ethanol to give 5-nitro-2-(2-hydroxyethylpiperazin-1-yl)benzonitrile (18.7 g), melting point 100–102° C.
Aufarbeitung
- customThe solvent was evaporated under reduced pressure
- additionTo the residue was added aqueous sodium hydroxide solution
- extractionthe mixture was extracted with chloroform
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customafter which the solvent was evaporated under reduced pressure
- additionTo the residue diisopropyl ether was added
- customcrystallization
- customThe crystals were recrystallized from hydrous ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-e9fb11f7b6aa4ae392142ff81f74b351
- Quelldatensatz
- uspto-grants-2006_03
- Patentnummer
- US07015218B1
Verknüpfte Notizen
Wird geladen…