Hydrochloric Acid → HCID 178444262、化合物

HRID 1936323ノート

反応式

HRID 1936323 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:7])[CH3:6].[CH2:9]([C@H:14]1[CH2:19][CH2:18][C@H:17]([C:20]2[CH:25]=[CH:24][C:23]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[CH:22][CH:21]=2)[CH2:16][CH2:15]1)[CH2:10][CH2:11][CH2:12][CH3:13].Cl>C(Cl)Cl>[C:5]([C:29]1[CH:30]=[CH:31][C:26]([C:23]2[CH:22]=[CH:21][C:20]([C@H:17]3[CH2:18][CH2:19][C@H:14]([CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH2:15][CH2:16]3)=[CH:25][CH:24]=2)=[CH:27][CH:28]=1)(=[O:7])[CH3:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 178444253HCID 178444253、化合物

生成物 1

HCID 178444262HCID 178444262、化合物収率 46.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

First, 23.6 g of anhydrous aluminum chloride and 120 ml of methylene chloride were put in a 300 ml flask. After 14.0 g of acetyl chloride was dropped into the mixture at 5° C. or less, the resultant mixture was stirred keeping the same temperature for 30 minutes. Then, 45.2 g of 4-(trans-4-pentylcyclohexyl)biphenyl was added to resultant mixture at 5° C. or less and stirred for 30 minutes at room temperature. After the reaction, the reaction solution was poured into dilute hydrochloric acid, and an organic layer was separated. The organic layer was then washed with water and dried with sodium sulfate. The solvent was then distilled off. The residue was recrystallized from acetone to obtain 24.0 g (Y: 46.0%) of 4-acetyl-4′-(trans-4-pentylcyclohexyl)biphenyl. The purity of the resultant compound was 99.7% as measured by GC.

後処理

  1. customfor 30 minutes
  2. customAfter the reaction
  3. customan organic layer was separated
  4. washThe organic layer was then washed with water
  5. dry with materialdried with sodium sulfate
  6. distillationThe solvent was then distilled off
  7. customThe residue was recrystallized from acetone

出典と根拠

ORDレコード
ord-c808bb0317524183bb7162557f29ab15
出典データセット
uspto-grants-2002_05
特許番号
US06388146B1

反応ノート

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