反应详情

4-{5-[4-(2-(Methanesulphonyl)ethyl)piperazin-1-yl]pyridin-2-yl}-3,4-dihydro-2H-quinoxaline-1-carboxylic acid tert-butyl ester (0.38 g, 0.76 mmol) is placed in 5 ml of dioxane and then 4N HCl in dioxane (2.84 ml, 11.36 mmol) is added. The reaction medium is stirred at ambient temperature for 18 h. 4N HCl in dioxane (2.84 ml, 11.36 mmol) is again added and the reaction medium is stirred at ambient temperature for an additional 18 h. After concentrating to dryness, the reaction medium is diluted with 50 ml of 1N HCl in water and extracted with 100 ml of diethyl ether. The organic phase is again washed with 50 ml of 1N HCl in water. The aqueous phases are combined, basified with K2CO3 powder up to a pH of 10 and extracted 3 times with 50 ml of dichloromethane. The resulting organic phases are combined, washed with a saturated aqueous sodium chloride solution, dried over MgSO4 and concentrated to dryness. 0.3 g of 1-{5-[4-(2-(methanesulphonyl)ethyl)piperazin-1-yl]pyridin-2-yl}-1,2,3,4-tetrahydroquinoxaline is obtained.

1. stirringthe reaction medium is stirred at ambient temperature for an additional 18 h
2. concentrationAfter concentrating to dryness
3. additionthe reaction medium is diluted with 50 ml of 1N HCl in water
4. extractionextracted with 100 ml of diethyl ether
5. washThe organic phase is again washed with 50 ml of 1N HCl in water
6. extractionextracted 3 times with 50 ml of dichloromethane
7. washwashed with a saturated aqueous sodium chloride solution
8. dry with materialdried over MgSO4
9. concentrationconcentrated to dryness