反応 #9581

反応方程式

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

収率 96.1%

溶媒

dichloromethane

反応条件

後処理

1. 1
   濃縮it was concentrated under reduced pressure
2. 2
   その他The resulting solid was isolated by filtration
3. 3
   濃縮concentrated under reduced pressure
4. 4
   その他The solid was then triturated with diethyl ether
5. 5
   その他isolated by filtration
6. 6
   その他An insoluble impurity was removed by filtration
7. 7
   濃縮the filtrate was concentrated under reduced pressure

実験手順

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.

出典