Chlorocyclohexane → Tricyclohexylbenzene

HRID 590894

반응식

HRID 590894 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

반응 조건

온도
3 °C

실험 절차

First, 6.83 g of aluminum chloride was added to 20.0 g of benzene, and agitated while cooling at 3° C. Then, 40.4 g of cyclohexyl chloride was slowly dropped thereinto. After the completion of the dropping, the mixture was agitated at room temperature for five hours and poured into ice water. The organic phase was extracted with ethyl acetate, and the obtained organic phase was subjected to vacuum distillation at 40° C. Further, vacuum distillation was performed at 170° C., and the product was cooled to room temperature. Thereafter, 50 ml of acetone was placed thereinto, and recrystallization was carried out. The resultant crystal was collected by filtration. Thus, 14 g of tricyclohexylbenzene was obtained.

후처리

  1. stirringAfter the completion of the dropping, the mixture was agitated at room temperature for five hours
  2. extractionThe organic phase was extracted with ethyl acetate
  3. distillationthe obtained organic phase was subjected to vacuum distillation at 40° C
  4. distillationFurther, vacuum distillation
  5. customwas performed at 170° C.
  6. temperaturethe product was cooled to room temperature
  7. customrecrystallization
  8. filtrationThe resultant crystal was collected by filtration

출처 및 근거

ORD 기록
ord-f89bd6f5c9d24abb8d5381c2aa50dcee
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09235116B2

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