Reaktionsgleichung
Cl.Cl[CH:3]([C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[CH:25]=[C:24]([CH3:26])[S:23][C:22]=1[CH3:27])[C:4]([N:6]([CH3:8])[CH3:7])=[O:5].C(S([O-])=O)O.[Na+]>ClCCl>[CH3:8][N:6]([CH3:7])[C:4](=[O:5])[CH2:3][C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[CH:25]=[C:24]([CH3:26])[S:23][C:22]=1[CH3:27]Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
34 g (0.077 mole) of α-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 500 ml of dichloromethane are treated with 36.9 g (0.24 mole) of Rongalite®, while stirring the mixture at room temperature for 24 h. The organic phase is separated after settling has taken place, the solid residue is washed with dichloromethane, the organic phase is washed with a saturated sodium hydrogen carbonate solution and then with water, it is dried over sodium sulphate, the solvent is evaporated under reduced pressure and 22 g of solid are obtained. After recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals are finally obtained. Melting point: 194°-195° C.
Aufarbeitung
- customThe organic phase is separated after settling
- washthe solid residue is washed with dichloromethane
- washthe organic phase is washed with a saturated sodium hydrogen carbonate solution
- dry with materialwith water, it is dried over sodium sulphate
- customthe solvent is evaporated under reduced pressure and 22 g of solid
- customare obtained
- customAfter recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals
- customare finally obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-d92df32fa3c24976935b2b186cc36c14
- Quelldatensatz
- uspto-grants-1995_05
- Patentnummer
- US05418248
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