Reaktionsgleichung
[CH3:1][N:2]([CH2:4][C:5]1[O:9][C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]([NH:20][CH3:21])=[CH:16][N+:17]([O-:19])=[O:18])=[CH:7][CH:6]=1)[CH3:3].[ClH:22]>C(OCC)(=O)C.C(O)(C)C>[ClH:22].[CH3:3][N:2]([CH2:4][C:5]1[O:9][C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]([NH:20][CH3:21])=[CH:16][N+:17]([O-:19])=[O:18])=[CH:7][CH:6]=1)[CH3:1]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
Under conditions of inert atmosphere, saturated with nitrogen, suspend 10.0 g of Z, N-[2-[[[5-(dimethylamino)methyl-2-furanyl]methyl]thio]ethyl]-N′-methyl-2-nitro-1,1-ethenediamine in 100 ml of anhydrous ethyl acetate (moisture<0.01%). Add dropwise to the mixture 21.95 g of hydrochloric acid in isopropanol (concentration 5.29% mol/mol) during 45 minutes, keeping the temperature at 25° C. Stirring vigorously, again in inert nitrogen atmosphere, a white precipitate is obtained. By operating again in a nitrogen-saturated atmosphere, wash and filter the precipitate with a mixture of ethyl acetate/isopropanol in 80:20 ratio and later with ethyl acetate alone. Dry the resulting precipitate in an oven at 40°-50° C. to remove the residual solvents and afterwards place it in a drier in-vacuo on phosphorus pentoxide, until a constant weight is obtained.
Aufarbeitung
- customat 25° C
- customa white precipitate is obtained
- washwash
- filtrationfilter the precipitate
- additionwith a mixture of ethyl acetate/isopropanol in 80:20 ratio
- customDry the resulting precipitate in an oven at 40°-50° C.
- customto remove the residual solvents
- customuntil a constant weight is obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-937d0cab4258481b85f85dcdb309c617
- Quelldatensatz
- uspto-grants-2005_02
- Patentnummer
- US06855835B2
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