تفاعل #65188

معادلة التفاعل

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

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر