HRID2414765

反应详情

EQUATION

反应方程式

HRID 2414765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

6-Nitro-4-chloro-2-(3-fluoro-phenyl)-quinoline, 20 g (59.4 mmoles), was placed in a 500 mL three-neck round-bottom flask equipped with magnetic stirrer, nitrogen inlet, gas outlet, condenser and heating bath. The material was dissolved in 150 mL of N-methyl pyrrolidinone, stirred and 250 mL of a 40% aq. solution of dimethylamine was added. The mixture was then warmed to 60° C. for 48 hrs. At the end of this time the reaction was cooled, poured into 3 L of water in a 4 L Erlenmeyer flask and the mixture stirred until solids formed. The solids were collected by vacuum filtration and dried in a vacuum oven. The product was recrystallised from-ethanol in a −20° C. freezer to give 19.6 g (95%) yield of the desired product.

WORKUP

后处理

  1. customequipped with magnetic stirrer, nitrogen inlet, gas outlet, condenser
  2. temperatureheating bath
  3. temperatureAt the end of this time the reaction was cooled
  4. stirringthe mixture stirred until solids
  5. customformed
  6. filtrationThe solids were collected by vacuum filtration
  7. customdried in a vacuum oven
  8. customThe product was recrystallised from-ethanol in a −20° C. freezer