Реакция #310787

ord-6b2686eae5fb440798c718571b3c8f2a

Уравнение реакции

CC1=CCC(C)C(C)C1=O
2,3,6-trimethylcyclohex-5-en-1-one
CN1CCCCC1
N-methylpiperidine
N
ammonia
[H][H]
hydrogen
CC1=CCC(C)C(C)C1=O
2,3,6-trimethyl-cyclohex-5-en-1-one
Cc1ccc(C)c(N)c1C
2,3,6-trimethylaniline

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  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
    Другоеproduced by the gas stream
  4. 4
    ДругоеThe reaction product is isolated
  5. 5
    Температураby cooling the exit gases
  6. 6
    workup.DISTILLATIONis distilled

Методика

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%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04355180uspto-grants-1982_10