Reaktion #65188

Reaktionsgleichung

α-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride

Rongalite

→

N,N-Dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]-benzothiazole-3-acetamide

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic phase is separated after settling
2. 2
   Waschenthe solid residue is washed with dichloromethane
3. 3
   Waschenthe organic phase is washed with a saturated sodium hydrogen carbonate solution
4. 4
   Trocknenwith water, it is dried over sodium sulphate
5. 5
   Sonstigethe solvent is evaporated under reduced pressure and 22 g of solid
6. 6
   Sonstigeare obtained
7. 7
   SonstigeAfter recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals
8. 8
   Sonstigeare finally obtained

Vorschrift

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.

Quelle