Acetone → N-(1,3-dithiol-2-ylidene)-N-methyl-N-(3-methylthio-1-ethoxycarbonylpropyl)ammonium perchlorate

HRID 648906Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 648906
CC(C)=O.[Cl:5]([O-:9])(=[O:8])(=[O:7])=[O:6].CS[C:12]1[S:16][CH:15]=[CH:14][S+:13]=1.C(OCC)C.[CH2:22]([O:24][C:25](=[O:33])[C@H:26]([CH2:29][CH2:30][S:31][CH3:32])[NH:27][CH3:28])[CH3:23]>C(OCC)(=O)C>[Cl:5]([O-:9])(=[O:8])(=[O:7])=[O:6].[S:16]1[CH:15]=[CH:14][S:13][C:12]1=[N+:27]([CH3:28])[CH:26]([C:25]([O:24][CH2:22][CH3:23])=[O:33])[CH2:29][CH2:30][S:31][CH3:32]

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 3283Diethyl EtherHCID 230390092-Methylthio-1,3-dithiolium perchlorateHCID 54331404Ethyl methyl-L-methioninate

Produkt 1

HCID 20144146N-(1,3-dithiol-2-ylidene)-N-methyl-N-(3-methylthio-1-ethoxycarbonylpropyl)ammonium perchlorateAusbeute 222,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To 100 ml of acetone, 2.0 g of 2-methylthio-1,3-dithiolium perchlorate was dissolved, and 50 ml of an ethyl ether solution containing 2.3 g of N-methyl methionine ethyl ester was gradually added thereto under stirring at room temperature. The mixture was stirred at room temperature for 6 hours, and then the solvent was distilled off. The residue was washed with ethyl acetate, whereby 7 g (yield: 54%) of N-(1,3-dithiol-2-ylidene)-N-methyl-N-(3-methylthio-1-ethoxycarbonylpropyl)ammonium perchlorate (Compound No. 6) was obtained as oily substance.

Aufarbeitung

  1. additionwas gradually added
  2. stirringThe mixture was stirred at room temperature for 6 hours
  3. distillationthe solvent was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-def2b37d134847c1a77ea87029718266
Quelldatensatz
uspto-grants-1988_04
Patentnummer
US04737494

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