HRID1534194

反应详情

EQUATION

反应方程式

HRID 1534194 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The atmosphere of a 500 ml eggplant flask equipped with a three-way cock at the top and an Allihn condenser was dried under reduced pressure and displaced with nitrogen. In the flask was charged 13.6 g (50 mmole) of 6,6'-dimethyl-2,2'-dinitro-1,1'-biphenyl (7) as obtained in Preparation Example 4 and dissolved in 120 ml of warm 99% ethanol having been previously displaced with nitrogen, followed by stirring. To the mixture was added 35 ml (0.7 mole) of hydrazine hydrate having been displaced with nitrogen. A suspension of 3 ml of a Raney nickel W2 type catalyst in ethanol was slowly added thereto by means of a syringe while maintaining the activity. Thereafter, the mixture was heated at reflux in an oil bath until the whole of the hydrazine was consumed.

WORKUP

后处理

  1. customThe atmosphere of a 500 ml eggplant flask equipped with a three-way cock at the top
  2. customan Allihn condenser was dried under reduced pressure
  3. customas obtained in Preparation Example 4
  4. additionwas slowly added
  5. temperatureby means of a syringe while maintaining the activity
  6. temperatureThereafter, the mixture was heated
  7. customwas consumed