반응 #9513

반응 방정식

(7-bromo-3-nitroquinolin-4-yl)-(4-chlorobutyl)amine

sodium hydrosulfite

→

7-bromo-N4-(4-chlorobutyl)quinoline-3,4-diamine

수율 98.0%

용매

methanol

water

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   기타The residue was partitioned between dichloromethane (300 mL) and aqueous sodium bicarbonate (150 mL of 50%)
3. 3
   기타The aqueous layer was separated
4. 4
   추출extracted with dichloromethane (2×50 mL)
5. 5
   건조The combined organic fractions were dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated under reduced pressure

실험 절차

A suspension of (7-bromo-3-nitroquinolin-4-yl)-(4-chlorobutyl)amine (8.05 g, 22.5 mmol) in methanol (250 mL) was cooled to 0° C.; a solution of sodium hydrosulfite (19.5 g, 112 mmol) in water (80 mL) was added dropwise over a period of 30 minutes. The reaction was stirred at ambient temperature for two hours and then concentrated under reduced pressure. The residue was partitioned between dichloromethane (300 mL) and aqueous sodium bicarbonate (150 mL of 50%). The aqueous layer was separated and extracted with dichloromethane (2×50 mL). The combined organic fractions were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 7.25 g of crude 7-bromo-N4-(4-chlorobutyl)quinoline-3,4-diamine as a light brown semi-solid.

출처