反应 #310787

ord-6b2686eae5fb440798c718571b3c8f2a

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITION1,000 parts by volume of catalyst are introduced into a fluidised bed reactor
  2. 2
    workup.WAITThe reactor is set to 230° C. and, per hour
  3. 3
    其他produced by the gas stream
  4. 4
    其他The reaction product is isolated
  5. 5
    温度by cooling the exit gases
  6. 6
    workup.DISTILLATIONis distilled

实验过程

1,000 parts by volume of catalyst are introduced into a fluidised bed reactor, having a capacity of 1.3 liters or 1,300 parts by volume. The catalyst consists of 0.5% by weight of Pd, 0.11% by weight of Zn and 0.1% by weight of Cd on Al2O3 and has a particle size of from 0.2 to 0.6 mm. The reactor is set to 230° C. and, per hour, a correspondingly preheated mixture of 200,000 parts by volume of ammonia and 10,000 parts by volume of hydrogen is passed in. Per hour, a solution of 50 parts of 2,3,6-trimethylcyclohex-5-en-1-one in 50 parts of N-methylpiperidine is sprayed continuously into the fluidised catalyst bed produced by the gas stream. The reaction product is isolated by cooling the exit gases, and is distilled. 100 parts of 2,3,6-trimethyl-cyclohex-5-en-1-one give 89 parts of 2,3,6-trimethylaniline; yield: 91%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04355180uspto-grants-1982_10