HRID2413152

反应详情

EQUATION

反应方程式

HRID 2413152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture was prepared from 10 g of 2-chloro-3-quinolinecarboxaldehyde, 5.2 g of hydroxylamine hydrochloride and 100 ml of phosphoryl chloride and heated with a heat lamp. The mixture was heterogeneous until the temperature reached 90° C. and there was no noticeable exotherm or gas evolution. After heating at reflux for 30 minutes, the mixture was cooled for 16 hours. It was then quenched in 700 ml of water. The tan solid which formed was separated by filtration and dried to give 7 g of crude 2-chloro-3-cyanoquinoline.

WORKUP

后处理

  1. temperatureheated with a heat lamp
  2. customreached 90° C.
  3. temperatureAfter heating
  4. temperatureat reflux for 30 minutes
  5. temperaturethe mixture was cooled for 16 hours
  6. customIt was then quenched in 700 ml of water
  7. customThe tan solid which formed
  8. customwas separated by filtration
  9. customdried