반응 #9483

반응 방정식

sodium hydrosulfite

potassium carbonate

tert-butyl[4-(7-bromo-3-nitroquinolin-4-ylamino)butyl]carbamate

→

tert-butyl[4-(3-amino-7-bromoquinolin-4-ylamino)butyl]carbamate

수율 99.0%

용매

water

dichloromethane

water

반응 조건

후처리

1. 1
   여과The reaction mixture was filtered through a layer of CELITE
2. 2
   여과filter aid
3. 3
   추출The aqueous filtrate was extracted with dichloromethane
4. 4
   건조the combined organic fractions were dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated under reduced pressure

실험 절차

A solution of sodium hydrosulfite (43.35 g, 249 mmol) and potassium carbonate (38.28 g, 277 mmol) in water (300 mL) was added to a mixture of tert-butyl[4-(7-bromo-3-nitroquinolin-4-ylamino)butyl]carbamate (24.3 g, 55.3 mmol) and 1,1′-diethyl-4,4′-bipyridinium dibromide (1.03 g, 2.76 mmol) in dichloromethane (368 mL) and water (40 mL), and the reaction was stirred overnight at ambient temperature. The reaction mixture was filtered through a layer of CELITE filter aid. The aqueous filtrate was extracted with dichloromethane, and the combined organic fractions were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 22.4 g of tert-butyl[4-(3-amino-7-bromoquinolin-4-ylamino)butyl]carbamate as a brown powder.

출처