Acetylsalicylic anhydride → HCID 13051192, Verbindung

HRID 904814Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 904814
C(OC1[C:6](=CC=CC=1)[C:7]([O:9][C:10](=[O:21])[C:11]1[C:12](=[CH:17][CH:18]=[CH:19][CH:20]=1)[O:13][C:14](=[O:16])[CH3:15])=O)(=O)C.OC(C)[CH2:28][N:29]1[CH2:34][CH2:33][N:32]([CH2:35][CH:36]([OH:38])[CH3:37])[CH2:31][CH2:30]1>C(OCC)(=O)C>[C:14]([O:13][C:12]1[C:11](=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]([O:9][CH:7]([CH3:6])[CH2:28][N:29]1[CH2:30][CH2:31][N:32]([CH2:35][CH:36]([O:38][C:10](=[O:9])[C:11]2[C:12](=[CH:17][CH:18]=[CH:19][CH:20]=2)[O:13][C:14](=[O:16])[CH3:15])[CH3:37])[CH2:33][CH2:34]1)=[O:21])(=[O:16])[CH3:15]

Komponenten

4

Edukt 2

HCID 15110Acetylsalicylic anhydrideHCID 966981,1'-(Piperazine-1,4-diyl)di(propan-2-ol)

Produkt 1

HCID 13051192HCID 13051192, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Dissolve acetylsalicylic anhydride (17.1 g; 0.05 moles) in an apolar organic solvent represented for example by ethyl acetate; add 1,4-bis-(2-hydroxypropyl)piperazine (5.06 g; 0.025 moles) to the solution, and heat up to the boiling point until the reaction is completed. After cooling at room temperature, wash the reaction mixture with a 5 percent aqueous solution of potassium carbonate, and then with water. Anhydrify the organic phase (K2CO3), filter, and treat it with anhydrous hydrochloric acid dissolved in diethylether causing by this procedure the precipitation of the raw product that, after collection and drying, can be recrystallized from a low molecular weight alcohol.

Aufarbeitung

  1. washwash the reaction mixture with a 5 percent aqueous solution of potassium carbonate
  2. filtrationAnhydrify the organic phase (K2CO3), filter
  3. additiontreat it with anhydrous hydrochloric acid
  4. dissolutiondissolved in diethylether causing by this procedure
  5. customthe precipitation of the raw product that
  6. customafter collection
  7. customdrying
  8. customcan be recrystallized from a low molecular weight alcohol

Quellen und Nachweise

ORD-Eintrag
ord-af88a6b3519a486b9b73a9dfb7f6e8f2
Quelldatensatz
uspto-grants-1983_12
Patentnummer
US04420482

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