Dimethyl Sulfoxide → HCID 86745743, Verbindung

HRID 1195243Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1195243
Cl.[CH:2]1([C:5]([C:7]2([CH3:10])[CH2:9][CH2:8]2)=[NH:6])[CH2:4]C1.[Cl:11]([O-:15])(=[O:14])(=[O:13])=[O:12].[NH4+].[CH3:17]S(C)=O>>[Cl:11]([O-:15])(=[O:14])(=[O:13])=[O:12].[NH3+:6][CH:5]1[C:7]2[CH2:9][CH2:8][CH2:17][C:10]=2[CH2:4][CH2:2]1

Komponenten

4

Edukt 3

HCID 679Dimethyl SulfoxideHCID 24639Ammonium perchlorateHCID 19819014HCID 19819014, Verbindung

Produkt 1

HCID 86745743HCID 86745743, VerbindungAusbeute 43 %

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of 1-cyclopropyl-1-(1-methylcyclopropyl)methanimine hydrochloride (0.060 g, 0.38 mmol) in 0.60 ml of dimethyl sulfoxide was added 0.088 g (0.75 mmol) of ammonium perchlorate. The mixture was heated with stirring at 100° C. for 20 hours. The solvent was distilled out in vacuo and ether was added to the residue. Precipitated crystals was obtained and recrystallized from ethanol to afford 0.36 g (Yield: 43%) of the desired compound.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-faae784c562345d58e00a7c07ea2c7c1
Quelldatensatz
uspto-grants-1992_05
Patentnummer
US05110945

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