Reaktion #65572

ord-01f89205b7bd469b9be2af90e59305c7

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe mixture is concentrated
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in ethyl ether
  3. 3
    WaschenThe solution is washed with diluted hydrochloric acid, aqueous sodium hydrogencarbonate solution and brine
  4. 4
    TrocknenThe organic layer is dried over sodium sulfate
  5. 5
    Filtrationfiltered off
  6. 6
    workup.DISTILLATIONThe filtrate is distilled away
  7. 7
    Sonstigethe resuling residue is crystallized

Vorschrift

To a solution of 0.82 g of 2-tert-butyl-6-methylaniline in pyridine is added a solution of 1.2 g of N-methyl-N-(2-phenylcyclohexyl)carbamoylchloride in dichloromethane dropwise. The mixture is stirred at room temperature until starting compounds disappear on TLC. The mixture is concentrated and the residue is dissolved in ethyl ether. The solution is washed with diluted hydrochloric acid, aqueous sodium hydrogencarbonate solution and brine. The organic layer is dried over sodium sulfate and filtered off. The filtrate is distilled away and the resuling residue is crystallized to give N-(2-tert-butyl-6-methylphenyl)-N'-methyl-N'-(2-phenylcyclohexyl)urea.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420164uspto-grants-1995_05