Reaktionsgleichung
[CH3:1][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH2:14])[N:9]=1)[CH3:3].[OH-].[Na+].[CH3:17][N:18]=[C:19](SC)[S:20][CH3:21]>C(O)C>[CH3:17][NH:18][C:19](=[N:14][CH2:13][CH2:12][S:11][CH2:10][C:8]1[N:9]=[C:5]([CH2:4][N:2]([CH3:1])[CH3:3])[S:6][CH:7]=1)[S:20][CH3:21]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
One g. of the oxalate salt of 2-dimethylaminomethyl-4-(2-aminoethyl)thiomethylthiazole was dissolved in 10 ml. of denatured ethanol and 4.8 ml. of 1N sodium hydroxide solution. To the mixture was added 0.36 g. of methylcarbonimidodithioic acid, dimethyl ester, and the reaction mixture was stirred under reflux for 16 hours. The mixture was then evaporated under vacuum, and the residue was taken up in 12 ml. of water and 1.5 ml. of 50% aqueous sodium hydroxide. The solution was extracted twice with 25 ml. portions of diethyl ether, and the organic layers were combined, dried over potassium carbonate and evaporated under vacuum to obtain 0.65 g. of the desired product in crude form. It was identified by nuclear magnetic resonance analysis as being identical to the product of Example 1.
Aufarbeitung
- additionTo the mixture was added 0.36 g
- temperatureunder reflux for 16 hours
- customThe mixture was then evaporated under vacuum
- extractionThe solution was extracted twice with 25 ml
- dry with materialdried over potassium carbonate
- customevaporated under vacuum
- customto obtain 0.65 g
Quellen und Nachweise
- ORD-Eintrag
- ord-2809c85ab34140b4b81bd03465a38bc8
- Quelldatensatz
- uspto-grants-1986_05
- Patentnummer
- US04587344
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