HRID745505

反应详情

EQUATION

反应方程式

HRID 745505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 0.62 g of 60% sodium hydride, 1.91 g of 3,6-dichloropyridazine and 10 ml of benzene was stirred while being cooled with ice, and a solution consisting of 1.32 g of 3-amino-3-methylbutanol, 3 ml of t-butanol and 5 ml of benzene was added dropwise. After stirring at room temperature for 30 minutes, ether was added to the reaction mixture, and the solid was removed by filtration with Hyflo Super-Cel. The filtrate was concentrated under reduced pressure. n-Hexane was added to the resulting oily product, and the mixture was allowed to stand to give 2.34 g of 3-(3-amino-3-methylbutoxy)-6-chloropyridazine as colorless crystals having a melting point of 63.5° to 65.0° C.

WORKUP

后处理

  1. temperaturewhile being cooled with ice
  2. additionwas added dropwise
  3. stirringAfter stirring at room temperature for 30 minutes
  4. customthe solid was removed by filtration with Hyflo Super-Cel
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. additionn-Hexane was added to the resulting oily product