반응 #1845692

ord-247a233a17c74811b356de9d8947fb00

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 1 hour
  2. 2
    workup.DISTILLATIONAfter distilling off the solvent
  3. 3
    세척washed
  4. 4
    workup.ADDITIONwith dilute alkaline solution and water
  5. 5
    workup.DISTILLATIONThe methylene chloride is distilled off
  6. 6
    기타the crude 2-(4-cyclohexylphenyl)imino-hexahydropyrimidine is recrystallised from acetonitrile

실험 절차

A solution of 2.9 g of N-(3-aminopropyl)-N'-(4-cyclohexylphenyl)thiourea and 0.65 ml of methyliodide in 20 ml of amyl alcohol is slowly heated to the boiling point and then refluxed for 1 hour. After distilling off the solvent, the residue is taken up in methylene chloride and washed with dilute alkaline solution and water. The methylene chloride is distilled off and the crude 2-(4-cyclohexylphenyl)imino-hexahydropyrimidine is recrystallised from acetonitrile. The purified product has a melting point of 179°-181° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04374143uspto-grants-1983_02