Hydrochloric Acid → 1-(4'-Methoxy(1,1'-biphenyl)-2-yl)ethan-1-one

HRID 2101231ノート

反応式

HRID 2101231 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.[Al+3].[Cl-].[Cl-].[Cl-].[C:19](Cl)(=[O:21])[CH3:20].Cl>O.C(=S)=S>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=2[C:19](=[O:21])[CH3:20])=[CH:5][CH:4]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 119434-MethoxybiphenylHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 43213891-(4'-Methoxy(1,1'-biphenyl)-2-yl)ethan-1-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6348Carbon Disulfide溶媒

実験手順

The 4′-methoxybiphenyl (0.05 mol) and AlCl3 (0.06 mol) were dissolved in boiling CS2 (60 mL) with stirring. Acetyl chloride (0.1 mol) was added dropwise and reflux continued for 1 hour. The mixture was poured onto crushed ice (150 mL) containing water (50 mL) and HCl (50 mL). The organic phase was separated and the CS2 removed by distillation. The residue was recrystallised from aqueous isopropanol to give the title compound. δC (CDCl3, 62.9 MHz): 26.6, 55.4, 114.4, 126.6, 128.4, 129.0, 132.2, 135.3, 145.4, 159.9 and 198.0

後処理

  1. temperaturereflux
  2. additionThe mixture was poured
  3. customThe organic phase was separated
  4. customthe CS2 removed by distillation
  5. customThe residue was recrystallised from aqueous isopropanol

出典と根拠

ORDレコード
ord-28c7f26a8ccf4af7a49217cf1aeb0d75
出典データセット
uspto-grants-2009_08
特許番号
US07572825B2

反応ノート

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