Sodium Carbonate → HCID 13236375, Verbindung

HRID 1649257Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1649257
[NH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH:8]=[CH:7]2.Br.[Br:14][CH2:15][CH2:16][NH:17][CH2:18][CH2:19]Br.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C>[BrH:14].[N:1]1([C:2]2[CH:3]=[CH:4][CH:5]=[C:6]3[C:11]=2[NH:10][C:9](=[O:12])[CH:8]=[CH:7]3)[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 12692731Ethanamine, 2-bromo-N-(2-bromoethyl)-, hydrobromide (1:1)HCID 133171128-Aminoquinolin-2(1H)-one

Produkt 1

HCID 13236375HCID 13236375, VerbindungAusbeute 17 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

8-Aminocarbostyril (15.47 g, 96.6 mmols) and bis(β-bromoethyl)amine hydrobromide (33 g, 106 mmols) were suspended in DMF and the suspension was stirred at 70° to 80° C. for 10 hours. After adding 5.1 g of sodium carbonate the reaction mixture was stirred at the same temperature as above for 7 hours. After distilling off the solvent under reduced pressure, methanol was added to the residue to crystallize. The crude crystals thus obtained were recrystallized from methanol-ether to give 5.1 g of 8-(1-piperazinyl)carbostyril hydrobromide, m.p. above 300° C., colorless scales.

Aufarbeitung

  1. stirringwas stirred at the same temperature as above for 7 hours
  2. distillationAfter distilling off the solvent under reduced pressure, methanol
  3. additionwas added to the residue
  4. customto crystallize
  5. customThe crude crystals thus obtained
  6. customwere recrystallized from methanol-ether

Quellen und Nachweise

ORD-Eintrag
ord-f59ee3fb5da545a8bae2259602b057d7
Quelldatensatz
uspto-grants-1983_11
Patentnummer
US04415572

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