Reaktionsgleichung
[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].CS[C:8]1[S:12][CH:11]=[CH:10][S+:9]=1.[CH2:13]([NH:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:14][CH2:15][CH3:16]>O1CCCC1>[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].[S:9]1[CH:10]=[CH:11][S:12][C:8]1=[N+:17]([CH2:18][CH2:19][CH2:20][CH3:21])[CH2:13][CH2:14][CH2:15][CH3:16]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To 10 ml of tetrahydrofuran, 2.0 g of 2-methylthio-1,3-dithiolium perchlorate was suspended, and 0.75 ml of dibutylamine was dropwise added over a period of 5 minutes. The mixture was stirred at room temperature for 30 minutes, and the solvent was distilled off under reduced pressure. The residue was dissolved in a mixture of acetone-ethyl ether, and cooled to -70° C. in a cooling medium, whereupon crystals precipitated. The crystals were collected by decantation under cooled condition, and purified by liquid chromatography (column: Senshu pack, Senshu ODS-5301, mobile phase: methanol/water=50/50), whereby 0.20 g (yield: 75%) of N-(1,3-dithiol-2-ylidene)-N,N-di(n-butyl)ammonium perchlorate was obtained as oily substance. (Compound No. 23)
Aufarbeitung
- distillationthe solvent was distilled off under reduced pressure
- dissolutionThe residue was dissolved in a mixture of acetone-ethyl ether
- temperaturecooled to -70° C. in a cooling medium, whereupon crystals
- customprecipitated
- customThe crystals were collected by decantation
- temperatureunder cooled condition
- custompurified by liquid chromatography (column: Senshu pack, Senshu ODS-5301, mobile phase: methanol/water=50/50)
Quellen und Nachweise
- ORD-Eintrag
- ord-3b5ce801c6e0432da8cca301aba6091e
- Quelldatensatz
- uspto-grants-1988_04
- Patentnummer
- US04737494
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