HRID1109433

反应详情

EQUATION

反应方程式

HRID 1109433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 12.0 g of 5-nitrosalicylaldehyde and 100 ml of chloromethyl methyl ether was cooled on an ice-bath and 43.9 g of anhydrous aluminum chloride was added in small portions. The mixture was stirred at room temperature for 10 minutes and, then, refluxed for 22 hours. This reaction mixture was cooled on an ice-bath and 200 ml of water was added with vigorous stirring, whereupon white crystals separated out. These white crystals are collected, dissolved in hot hexane and filtered and the mother liquor was cooled to give 14.9 g of 3-chloromethyl-5-nitrosalicylaldehyde as colorless needles (Yield 72%).

WORKUP

后处理

  1. temperaturewas cooled on an ice-bath
  2. temperaturerefluxed for 22 hours
  3. temperatureThis reaction mixture was cooled on an ice-bath
  4. customseparated out
  5. customThese white crystals are collected
  6. dissolutiondissolved in hot hexane
  7. filtrationfiltered
  8. temperaturethe mother liquor was cooled