Sodium Bicarbonate → HCID 13231125, Verbindung

HRID 905029Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 905029
[C:1]([CH2:9][CH2:10][CH2:11][CH2:12]Br)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:14]([O:16][C:17]([NH:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)=[O:18])[CH3:15].C(=O)([O-])O.[Na+]>C(O)C>[C:1]([CH2:9][CH2:10][CH2:11][CH2:12][N:23]1[CH2:22][CH2:21][N:20]([NH:19][C:17]([O:16][CH2:14][CH3:15])=[O:18])[CH2:25][CH2:24]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 111840715-bromo-1-phenyl-1-pentanoneHCID 13200156Ethyl piperazin-1-ylcarbamate

Produkt 1

HCID 13231125HCID 13231125, VerbindungAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

17.0 g of 1-benzoyl-4-bromobutane, 13.4 g of 1-(ethoxycarbonylamino)piperazine and 17.8 g of sodium hydrogen carbonate were heated under reflux in ethanol for 6 hours with stirring. The insoluble materials were removed from the reaction mixture by filtration. The solvent was distilled off, and water was added to the residue. The mixture was extracted with benzene. The extract was recrystallized from benzene-hexane to give 21.4 g of 4-(4-benzoylbutyl)-1-(ethoxycarbonylamino)-piperazine having a melting point of 105° to 106° C.

Aufarbeitung

  1. customThe insoluble materials were removed from the reaction mixture by filtration
  2. distillationThe solvent was distilled off
  3. additionwater was added to the residue
  4. extractionThe mixture was extracted with benzene
  5. customThe extract was recrystallized from benzene-hexane

Quellen und Nachweise

ORD-Eintrag
ord-6ade663aa5af422791a2999fdf531c7d
Quelldatensatz
uspto-grants-1983_12
Patentnummer
US04421754

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