HRID1818231

反应详情

EQUATION

反应方程式

HRID 1818231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. concentrationit was concentrated under reduced pressure
  2. customThe resulting solid was isolated by filtration
  3. concentrationconcentrated under reduced pressure
  4. customThe solid was then triturated with diethyl ether
  5. customisolated by filtration
  6. customAn insoluble impurity was removed by filtration
  7. concentrationthe filtrate was concentrated under reduced pressure