HRID606118

反应详情

EQUATION

反应方程式

HRID 606118 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under a nitrogen atmosphere, acetonitrile (1.5 L) was added to a Parr vessel containing 5% platinum on carbon (1.5 g), which had been wet with a small amount of acetonitrile, and 2-chloro-N-{2-[3-(4-fluorophenyl)isoxazol-5-yl]ethyl}-3-nitroquinolin-4-amine (23.20 g, 56.20 mmol). The vessel was sealed, purged three times with hydrogen, and placed under hydrogen pressure (30 psi, 2.1×105 Pa) for 18 hours at room temperature. The catalyst was removed by filtration, and the majority of the filtrate was concentrated under reduced pressure. A solid was present in the remaining filtrate and was isolated by filtration to provide 11.3 g of 2-chloro-N4-{2-[3-(4-fluorophenyl)isoxazol-5-yl]ethyl}quinoline-3,4-diamine as a yellow solid.

WORKUP

后处理

  1. customThe vessel was sealed
  2. custompurged three times with hydrogen
  3. customfor 18 hours
  4. customat room temperature
  5. customThe catalyst was removed by filtration
  6. concentrationthe majority of the filtrate was concentrated under reduced pressure
  7. customwas isolated by filtration