反応 #1483143

ord-87c240b571e64296b893c4fef78630b5

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 5 hours
  2. 2
    抽出An organic layer was extracted by use of ethyl acetate
  3. 3
    workup.DISTILLATIONthe obtained organic layer was distilled at 40° C. under reduced pressure and further at 170° C. under reduced pressure
  4. 4
    温度The resultant matter was cooled to room temperature
  5. 5
    workup.ADDITION50 ml of acetone was poured
  6. 6
    その他recrystallization
  7. 7
    その他The crystal obtained by the recrystallization
  8. 8
    ろ過was collected by filtration

実験手順

Aluminum chloride amounting to 6.83 g 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 5 hours and poured into ice water. An organic layer was extracted by use of ethyl acetate, and the obtained organic layer was distilled at 40° C. under reduced pressure and further at 170° C. under reduced pressure. The resultant matter was cooled to room temperature, and 50 ml of acetone was poured thereinto to thereby carry out recrystallization. The crystal obtained by the recrystallization was collected by filtration. Thus, 14 g of tricyclohexylbenzene was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08900791B2uspto-grants-2014_12