반응 #69970

반응 방정식

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

용매

dichloromethane

dioxane

반응 조건

후처리

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

실험 절차

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.

출처