HRID963421

反应详情

EQUATION

反应方程式

HRID 963421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2 g of di-2-pyridyl-ketone and 1.51 g of hydroxylamine-hydrochloride are added to 13 ml of pyridine and the mixture is held at reflux for 4 hrs. After concentration and cooling there are isolated 2.95 g of crude di-2-pyridyl ketone oxime (contaminated with salts). Addition of 1.18 g of ammonium acetate, 44 ml of dil. ammonia, 30 ml of water and 30 ml of ethanol yields a suspension which is treated portionwise with 4.5 g of zinc powder. The mixture is held at reflux for 4 hrs., cooled and suction filtered. The filtrate is concentrated and the residue is triturated with methanol. 2.54 g of crude C,C-dipyridin-2-yl-methylamine are isolated. Yield: 93%.

WORKUP

后处理

  1. temperatureat reflux for 4 hrs
  2. concentrationAfter concentration
  3. temperaturecooling there