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

HRID 1195236Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1195236
Cl.[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 19819017HCID 19819017, Verbindung

Produkt 1

HCID 10878400Pyrrolizinium, 1,2,3,5,6,7-hexahydro-, perchlorateAusbeute 400,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of dicyclopropylmethanimine hydrochloride (1.00 g, 6.87 mmol) in 6.0 ml of dimethyl sulfoxide was added 1.68 g (1.37 mmol) of ammonium perchlorate. The mixture was heated with stirring at 100° C. for 6 hours. The solvent was distilled out in vacuo and isobutyl alcohol (6 ml) was added to the residue. Precipitated crystals was obtained and recrystallized from ethanol to afford 1.15 g (Yield: 80%) of the desired compound.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-e7af98f8f1474f33bb6573eff90da3f5
Quelldatensatz
uspto-grants-1992_05
Patentnummer
US05110945

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