HRID26362

反应详情

EQUATION

反应方程式

HRID 26362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture consisting of 128 g (1.0 mole) of o-chloroaniline, 304 g of conc. hydrochloric acid and 61 g of water was maintained at 90°-95° C., and with sufficient stirring, 70 g (1.0 mole) of crotonaldehyde was added dropwise over the course of 2 hours. After the addition, the mixture was reacted further at 90°-95° C. for 1 hour. The reaction mixture was cooled, and then rendered alkaline by adding a conc. aqueous solution containing 132 g of sodium hydroxide with ice cooling. The alkaline mixture was separated into layers, and the oily layer was distilled at 2-3 mmHg to afford 72 g (0.4 mole) of 8-chloroquinaldine.

WORKUP

后处理

  1. temperaturewas maintained at 90°-95° C.
  2. additionAfter the addition
  3. customthe mixture was reacted further at 90°-95° C. for 1 hour
  4. temperatureThe reaction mixture was cooled
  5. additionby adding a conc. aqueous solution
  6. customThe alkaline mixture was separated into layers
  7. distillationthe oily layer was distilled at 2-3 mmHg