Acetic Anhydride → HCID 21409820, Verbindung

HRID 1283539Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1283539
[NH2:1][CH2:2][C:3]1([N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[C:16](OC(=O)C)(=[O:18])[CH3:17]>>[C:16]([NH:1][CH2:2][C:3]1([N:9]2[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH2:14]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)(=[O:18])[CH3:17]

Komponenten

3

Edukt 2

HCID 7918Acetic AnhydrideHCID 70181321-[1-(4-METHYLPIPERAZIN-1-YL)CYCLOHEXYL]METHANAMINE

Produkt 1

HCID 21409820HCID 21409820, VerbindungAusbeute 65 %

Versuchsvorschrift

1-[1-(Aminomethyl)cyclohexyl]-4-methyl piperazine (10.57 g.,) was added slowly to stirred acetic anhydride (40 ml) cooled in ice and the stirring was continued for 15 mins. The mixture was heated under reflux for 1 hr.. The solution was evaporated to dryness and re-evaporated with ethanol/benzene (X2). The residue was dissolved in water, the solution made alkaline with 5NNaOH (pH = 14), extracted with chloroform (X3), dried (anhyd.Na2SO4) and evaporated. The residue was dissolved in hot petroleum ether (80°-100°) decolourised with charcoal and allowed to cool. The crystalline solid which formed was recrystallised from petroleum ether (b.p. 80°-100°) to give 1-[1-(acetamidomethyl)cyclohexyl]-4-methyl piperazine (8.3 g; 65%) m.p. 110°-111°.

Aufarbeitung

  1. temperaturecooled in ice
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 1 hr
  4. customThe solution was evaporated to dryness
  5. customre-evaporated with ethanol/benzene (X2)
  6. dissolutionThe residue was dissolved in water
  7. extractionextracted with chloroform (X3)
  8. dry with materialdried (anhyd.Na2SO4)
  9. customevaporated
  10. dissolutionThe residue was dissolved in hot petroleum ether (80°-100°)
  11. temperatureto cool
  12. customThe crystalline solid which formed
  13. customwas recrystallised from petroleum ether (b.p. 80°-100°)

Quellen und Nachweise

ORD-Eintrag
ord-950b179b730d4b9b803d8ad109ca1f23
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03975443

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