反応 #65572

ord-01f89205b7bd469b9be2af90e59305c7

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The mixture is concentrated
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in ethyl ether
  3. 3
    洗浄The solution is washed with diluted hydrochloric acid, aqueous sodium hydrogencarbonate solution and brine
  4. 4
    乾燥The organic layer is dried over sodium sulfate
  5. 5
    ろ過filtered off
  6. 6
    workup.DISTILLATIONThe filtrate is distilled away
  7. 7
    その他the resuling residue is crystallized

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05420164uspto-grants-1995_05