HRID2296501

反应详情

EQUATION

反应方程式

HRID 2296501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
230 °C

PROCEDURE

实验过程

1.650 kg of 2,6-dimethylphenol and 150 g of a pulverulent catalyst which contains 5.0% by weight of palladium and 2.5% by weight of praseodymium oxide, the remainder being aluminum oxide, are introduced into a 10 l stirred autoclave. The autoclave is closed and 1.370 kg of ammonia are forced in. The mixture is then heated to 230° C. and a pressure of 200 bar is established by forcing in hydrogen. The mixture is kept at the reaction temperature until a constant pressure is achieved (about 8 hours). It is then left to cool, and is filtered to give 1.710 kg of crude 2,6-dimethylcyclohexylamine (a mixture of 3 stereoisomeric 2,6-dimethylcyclohexylamines). The crude product is distilled to give 1.685 kg of 2,6-dimethylcyclohexylamine, boiling point=167°-168° C., corresponding to a yield of 98%.

WORKUP

后处理

  1. additionare introduced into a 10 l
  2. customThe autoclave is closed
  3. custom(about 8 hours)
  4. waitIt is then left
  5. temperatureto cool
  6. filtrationis filtered