반응 #9581

반응 방정식

7-Bromo-4-chloro-3-nitroquinoline

(S)-2,2-dimethyl-[1,3]dioxolane-4-methanamine

ethanol

→

(S)-(7-bromo-3-nitroquinolin-4-yl)-(2,2-dimethyl-1,3-dioxolan-4-ylmethyl)amine

수율 96.1%

용매

dichloromethane

반응 조건

후처리

1. 1
   농축it was concentrated under reduced pressure
2. 2
   기타The resulting solid was isolated by filtration
3. 3
   농축concentrated under reduced pressure
4. 4
   기타The solid was then triturated with diethyl ether
5. 5
   기타isolated by filtration
6. 6
   기타An insoluble impurity was removed by filtration
7. 7
   농축the filtrate was concentrated under reduced pressure

실험 절차

7-Bromo-4-chloro-3-nitroquinoline (11.00 g, 38.26 mmol) was reacted with (S)-2,2-dimethyl-[1,3]dioxolane-4-methanamine (5.81 g, 57.4 mmol) according to the method described in Part A of Examples 125–135. When the reaction was complete, it was concentrated under reduced pressure, and the residue was stirred with water (100 mL). The resulting solid was isolated by filtration, mixed twice with ethanol and concentrated under reduced pressure. The solid was then triturated with diethyl ether, isolated by filtration, and dissolved in dichloromethane. An insoluble impurity was removed by filtration, and the filtrate was concentrated under reduced pressure to provide 14.05 g of (S)-(7-bromo-3-nitroquinolin-4-yl)-(2,2-dimethyl-1,3-dioxolan-4-ylmethyl)amine as a yellow solid.

출처