Diethyl Ether → 3-(4-Biphenylyl)-4-(4-chlorophenyl)-2-butanone

HRID 52853ノート

反応式

HRID 52853 の反応式
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([CH2:7][C:8](=[O:10])[CH3:9])=[CH:3][CH:2]=1.[Cl:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22]Cl)=[CH:20][CH:19]=1.[OH-].[Na+].C(OCC)C>O>[C:1]1([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:2]=[CH:3][C:4]([CH:7]([CH2:22][C:21]2[CH:24]=[CH:25][C:18]([Cl:17])=[CH:19][CH:20]=2)[C:8](=[O:10])[CH3:9])=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 14798Sodium HydroxideHCID 2193711-Biphenyl-4-yl-propan-2-one

生成物 1

HCID 190737923-(4-Biphenylyl)-4-(4-chlorophenyl)-2-butanone収率 53.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

9.93 g of 1-(4-biphenylyl)-2-propanone, 8.4 g of 4chlorobenzyl chloride and 2.1 g of sodium hydroxide were mixed and heated for 5 hours with stirring on an oil bath of 80° to 90° C. The reaction solution was left to cool to room temperature. Then, ethyl ether and water were added thereto. The organic layer was collected by separation and then dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and then the solvent was distilled off under reduced pressure. The residue was recrystallized from hexane to obtain 8.42 g (yield: 53%) of the above-identified compound as colorless needles having a melting point of from 107 to 108.5° C.

後処理

  1. temperatureheated for 5 hours
  2. waitThe reaction solution was left
  3. customThe organic layer was collected by separation
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe drying agent was separated by filtration
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was recrystallized from hexane

出典と根拠

ORDレコード
ord-855491279dc34b29b593d6662b82a7fc
出典データセット
uspto-grants-1997_04
特許番号
US05616803

反応ノート

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