Chlorocyclohexane → Tricyclohexylbenzene

HRID 926441

反応式

HRID 926441 の反応式
[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

参加物

4

反応物 2

HCID 10952ChlorocyclohexaneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 3015433Tricyclohexylbenzene収率 50.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
3 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-07539820e33d4892b166061072dcd109
出典データセット
uspto-grants-2016_03
特許番号
US09285679B2

関連ノート

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