HRID1992604

反应详情

EQUATION

反应方程式

HRID 1992604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 7-bromo-4-chloro-3-nitroquinoline (10.00 g, 34.78 mmol) in dichloromethane (140 mL) was added triethylamine (10.2 mL, 73.1 mmol). The solution was cooled to 0° C., and 3-amino-1-butanol (2.80 mL, 36.5 mmol) was added. The solution was stirred overnight at ambient temperature and then filtered to collect a precipitate. The precipitate was washed with dichloromethane and water. The filtrate was washed with saturated aqueous sodium bicarbonate and then added to the precipitate. The mixture was concentrated under reduced pressure. Methanol and toluene were added several times and removed under reduced pressure. The resulting solid was dried under high vacuum to provide 11.34 g of 3-[(7-bromo-3-nitroquinolin-4-yl)amino]propan-1-ol as a yellow solid.

WORKUP

后处理

  1. filtrationfiltered
  2. customto collect a precipitate
  3. washThe precipitate was washed with dichloromethane and water
  4. washThe filtrate was washed with saturated aqueous sodium bicarbonate
  5. additionadded to the precipitate
  6. concentrationThe mixture was concentrated under reduced pressure
  7. additionMethanol and toluene were added several times
  8. customremoved under reduced pressure
  9. customThe resulting solid was dried under high vacuum