Ammonium perchlorate → Pyrrolizinium, 1,2,3,5,6,7-hexahydro-, perchlorate

HRID 1195237Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1195237
Br.[CH:2]1([C:5]([CH:7]2[CH2:9][CH2:8]2)=[NH:6])[CH2:4][CH2:3]1.[Cl:10]([O-:14])(=[O:13])(=[O:12])=[O:11].[NH4+]>CS(C)=O>[Cl:10]([O-:14])(=[O:13])(=[O:12])=[O:11].[N+:6]12[CH2:9][CH2:8][CH2:7][C:5]=1[CH2:2][CH2:3][CH2:4]2

Komponenten

4

Edukt 2

HCID 24639Ammonium perchlorateHCID 19819013HCID 19819013, Verbindung

Produkt 1

HCID 10878400Pyrrolizinium, 1,2,3,5,6,7-hexahydro-, perchlorateAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of dicyclopropylmethanimine hydrobromide (1.00 g, 5.26 mmol) in 6.0 ml of dimethyl sulfoxide was added 1.29 g (10.5 mmol) of ammonium perchlorate. The mixture was heated with stirring at 100° C. for 1 hour. The solvent was distilled out in vacuo and isobutyl alcohol was added to the residue. Precipitated crystals was obtained and recrystallized from ethanol to afford 0.90 g (Yield: 82%) of the desired compound.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. distillationThe solvent was distilled out in vacuo and isobutyl alcohol
  3. additionwas added to the residue
  4. customPrecipitated crystals
  5. customwas obtained
  6. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-96ec4aa98ca345209bdca8f0a32053a8
Quelldatensatz
uspto-grants-1992_05
Patentnummer
US05110945

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