反応 #65188

反応方程式

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

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The organic phase is separated after settling
2. 2
   洗浄the solid residue is washed with dichloromethane
3. 3
   洗浄the organic phase is washed with a saturated sodium hydrogen carbonate solution
4. 4
   乾燥with water, it is dried over sodium sulphate
5. 5
   その他the solvent is evaporated under reduced pressure and 22 g of solid
6. 6
   その他are obtained
7. 7
   その他After recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals
8. 8
   その他are finally obtained

実験手順

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.

出典