Chlorocyclohexane → Tricyclohexylbenzene

HRID 1185987

反応式

HRID 1185987 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

To 20.0 g of benzene, 6.83 g of aluminum chloride was added, cooled by 3° C. and stirred, and 40.4 g of cyclohexyl chloride was slowly added dropwise. After the dropwise addition, the mixture was stirred for 5 hours at room temperature and was poured into ice water. An organic phase was extracted using ethyl acetate and the obtained organic phase was distilled off at reduced pressure at 40° C. After further distilling off at reduced pressure at 170° C., the organic phase was cooled to room temperature, 50 ml of acetone was introduced and recrystallized. The precipitated crystals were filtered off and 14 g of tricyclohexylbenzene was obtained.

後処理

  1. additionAfter the dropwise addition
  2. stirringthe mixture was stirred for 5 hours at room temperature
  3. extractionAn organic phase was extracted
  4. distillationthe obtained organic phase was distilled off at reduced pressure at 40° C
  5. distillationAfter further distilling off at reduced pressure at 170° C.
  6. temperaturethe organic phase was cooled to room temperature
  7. addition50 ml of acetone was introduced
  8. customrecrystallized
  9. filtrationThe precipitated crystals were filtered off

出典と根拠

ORDレコード
ord-15212c28defa4df88e6588c79f58b0b5
出典データセット
uspto-grants-2014_03
特許番号
US08673538B2

関連ノート

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