تفاعل #65574

ord-03085be664434eebbe7e6fc4b41d7bde

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with ethyl acetate
  2. 2
    غسيلThe extract was washed with water, aqueous sodium hydrogencarbonate solution and saturated brine
  3. 3
    تجفيفdried over magnesium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled away in vacuo
  5. 5
    أخرىto give 2 g of crude crystals
  6. 6
    أخرىThe crystals were recrystallized from the mixture of ethyl acetate and hexane

الإجراء التجريبي

To the solution of 2 g of N-(4-phenylcyclohexyl)-N-cyclohexylmethylamine in dichloromethane was added 2 ml of pyridine and to the mixture was added a solution of 1.6 g of 2,6-diethylphenylisocyanate in 30 ml of dichloromethane dropwise. After the mixture was stirred at room temperature, to the solution was added diluted hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, aqueous sodium hydrogencarbonate solution and saturated brine and then dried over magnesium sulfate. The solvent was distilled away in vacuo to give 2 g of crude crystals. The crystals were recrystallized from the mixture of ethyl acetate and hexane to give 1.2 g of N-(2,6-diethylphenyl)-N'-cyclohexylmethyl-N'-(4-phenylcyclohexyl)urea, melting at 166°-168° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05420164uspto-grants-1995_05