반응 #65188

반응 방정식

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

용매

dichloromethane

반응 조건

후처리

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

실험 절차

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.

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