反応 #678076

ord-f89bd6f5c9d24abb8d5381c2aa50dcee

溶媒

反応条件

温度
3°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGAfter the completion of the dropping, the mixture was agitated at room temperature for five hours
  2. 2
    抽出The organic phase was extracted with ethyl acetate
  3. 3
    workup.DISTILLATIONthe obtained organic phase was subjected to vacuum distillation at 40° C
  4. 4
    workup.DISTILLATIONFurther, vacuum distillation
  5. 5
    その他was performed at 170° C.
  6. 6
    温度the product was cooled to room temperature
  7. 7
    その他recrystallization
  8. 8
    ろ過The resultant crystal was collected by filtration

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09235116B2uspto-grants-2016_01