تفاعل #69970

ord-2ae001ada5f2421ab344445f73fa6188

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530657B2uspto-grants-2013_09