Chlorocyclohexane → Tricyclohexylbenzene

HRID 926441

반응식

HRID 926441 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH:5]1(Cl)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1>C1C=CC=CC=1>[CH:5]1([C:5]2[C:6]([CH:5]3[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]3)=[C:7]([CH:5]3[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]3)[CH:8]=[CH:9][CH:10]=2)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1

참가 물질

4

반응물 2

HCID 10952ChlorocyclohexaneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 3015433Tricyclohexylbenzene수율 50.7%

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
3 °C

실험 절차

6.83 g of aluminum chloride was added to 20.0 g of benzene, followed by cooling/stirring at 3° C., and 40.4 g of cyclohexyl chloride was slowly added dropwise. After the dropwise addition, the mixture was stirred at room temperature for 5 hours and poured into ice water. The organic layer was extracted with ethyl acetate, and the obtained organic layer was distilled off under reduced pressure at 40° C. After further distillation off under reduced pressure at 170° C., the product was cooled to room temperature, charged into 50 ml of acetone and thereby recrystallized. The crystal precipitated was collected by filtration to obtain 14 g of tricyclohexylbenzene.

후처리

  1. additionAfter the dropwise addition
  2. stirringthe mixture was stirred at room temperature for 5 hours
  3. extractionThe organic layer was extracted with ethyl acetate
  4. distillationthe obtained organic layer was distilled off under reduced pressure at 40° C
  5. distillationAfter further distillation off under reduced pressure at 170° C.
  6. temperaturethe product was cooled to room temperature
  7. additioncharged into 50 ml of acetone
  8. customrecrystallized
  9. customThe crystal precipitated
  10. filtrationwas collected by filtration

출처 및 근거

ORD 기록
ord-07539820e33d4892b166061072dcd109
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09285679B2

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