Reaktion #69970

Reaktionsgleichung

hydrochloric acid

4-[4-(4-(methanesulphonyl)piperazin-1-yl)phenyl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid

→

1-[4-(4-(methanesulphonyl)piperazin-1-yl)phenyl]-1,2,3,4-tetrahydroquinoxaline

Lösungsmittel

dichloromethane

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solvents are evaporated under reduced pressure
2. 2
   workup.ADDITIONWater, a saturated aqueous sodium hydrogencarbonate solution and dichloromethane are added
3. 3
   ExtraktionThe aqueous sodium phase is extracted twice with dichloromethane
4. 4
   Waschenwashed with water
5. 5
   Trocknendried over magnesium sulphate
6. 6
   Sonstigethe solvent is evaporated under reduced pressure

Vorschrift

31.5 g of the tert-butyl ester of 4-[4-(4-(methanesulphonyl)piperazin-1-yl)phenyl]-3,4-dihydro-2H-quinoxaline-1-carboxylic acid are placed in 400 ml of dichloromethane and then 333 ml of 4N hydrochloric acid in dioxane are added. After stirring for 16 h under an inert atmosphere, the solvents are evaporated under reduced pressure. Water, a saturated aqueous sodium hydrogencarbonate solution and dichloromethane are added. The aqueous sodium phase is extracted twice with dichloromethane. The organic phases are combined, washed with water and dried over magnesium sulphate and then the solvent is evaporated under reduced pressure. 23.2 g of 1-[4-(4-(methanesulphonyl)piperazin-1-yl)phenyl]-1,2,3,4-tetrahydroquinoxaline are obtained. The product is subsequently used as is without other purification.

Quelle