Piperazine → N-[4-(1-Piperazinyl)butyl]-3,3-dimethylglutarimide

HRID 2199046

Reaktionsgleichung

Reaktionsgleichung von HRID 2199046
Br[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]1=[O:15].CC1(C)CC(=O)NC(=O)C1.[NH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[N:26]1([CH2:2][CH2:3][CH2:4][CH2:5][N:6]2[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]2=[O:15])[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1

Komponenten

6

Edukt 4

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 142924,4-Dimethylpiperidine-2,6-dioneHCID 136603351-(4-Bromobutyl)-4,4-dimethylpiperidine-2,6-dione

Produkt 1

HCID 20516935N-[4-(1-Piperazinyl)butyl]-3,3-dimethylglutarimideAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A mixture of N-(4-bromobutyl)-3,3-dimethylglutarimide (20.0 g; 0.07 mole [prepared from 3,3-dimethylglutarimide using the method of Example 2]); piperazine (31.0 g; 0.36 mole); K2CO3 (29.8 g; 0.22 mole); and KI (0.1 g) was refluxed in 250 mL acetonitrile for 18 hr. The mixture was filtered, concentrated and the unreacted piperazine removed by vacuum sublimation. The residual material was distilled to yield 17.2 g (85%) product, b.p. 170°-178° C. at 0.01 mm.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customthe unreacted piperazine removed by vacuum sublimation
  4. distillationThe residual material was distilled

Quellen und Nachweise

ORD-Eintrag
ord-613b4dba2a814f92b4367ed0edb4cfd4
Quelldatensatz
uspto-grants-1982_11
Patentnummer
US04361565

Verknüpfte Notizen

Wird geladen…