반응 #2122506

ord-21951efda33b4875984a232e3799e524

반응 방정식

[Al+3].[Cl-].[Cl-].[Cl-]
Aluminum chloride
ClC1CCCCC1
cyclohexyl chloride
c1cc(C2CCCCC2)c(C2CCCCC2)c(C2CCCCC2)c1
tricyclohexylbenzene
수율 50.7%

용매

반응 조건

온도
3°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    workup.STIRRINGthe resultant was stirred at room temperature for 5 hours
  3. 3
    기타the obtained reaction solution
  4. 4
    추출The organic layer was extracted
  5. 5
    기타the obtained organic layer was removed by distillation at 40° C. under reduced pressure
  6. 6
    기타The resultant was further removed by distillation at 170° C. under reduced pressure
  7. 7
    온도cooled to room temperature
  8. 8
    workup.ADDITION50 ml of acetone was added
  9. 9
    기타recrystallization
  10. 10
    기타The precipitated crystals were collected
  11. 11
    여과through filtering

실험 절차

Aluminum chloride (6.38 g) was added to 20.0 g of benzene, followed by stirring under cooling at 3° C., and 40.4 g of cyclohexyl chloride was slowly added dropwise thereto. After the dropwise addition, the resultant was stirred at room temperature for 5 hours, and the obtained reaction solution was added to ice water. The organic layer was extracted by using ethyl acetate, and the obtained organic layer was removed by distillation at 40° C. under reduced pressure. The resultant was further removed by distillation at 170° C. under reduced pressure and then cooled to room temperature, and 50 ml of acetone was added thereto to cause recrystallization. The precipitated crystals were collected through filtering, thereby obtaining 14 g of tricyclohexylbenzene.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08574814B2uspto-grants-2013_11