Methanol → Methyl 4-(4-chloro-1-oxobutyl)-alpha,alpha-dimethylbenzeneacetate

HRID 411908ノート

反応式

HRID 411908 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([OH:16])=[O:15])=[CH:9][CH:8]=1)=[O:6].[CH3:19]O>Cl>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([O:16][CH3:19])=[O:15])=[CH:9][CH:8]=1)=[O:6]

参加物

4

反応物 2

HCID 887MethanolHCID 109235672-(4-(4-Chlorobutanoyl)phenyl)-2-methylpropanoic acid

生成物 1

HCID 10062338Methyl 4-(4-chloro-1-oxobutyl)-alpha,alpha-dimethylbenzeneacetate収率 95.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒2 回

実験手順

Dissolve 2-[4-(4-chloro-butyryl)-phenyl]-2-methyl-propionic acid (6.2 g, 23.1 mmol) in hot methanolic solution of anhydrous hydrogen chloride (42 mL of a methanol containing 3.2 g of anhydrous hydrogen chloride). Reflux for 42 minutes, evaporate the solvent in vacuo, dissolve the residue in methylene chloride and wash with water. Dry (MgSO4), filter through silica gel, washing the gel with methylene chloride. Combine the organic washings and evaporate the solvent in vacuo to give the title compound as a clear oil (6.21 g, 94%).

後処理

  1. temperatureReflux for 42 minutes
  2. customevaporate the solvent in vacuo
  3. dissolutiondissolve the residue in methylene chloride
  4. washwash with water
  5. dry with materialDry (MgSO4)
  6. filtrationfilter through silica gel
  7. washwashing the gel with methylene chloride
  8. customevaporate the solvent in vacuo

出典と根拠

ORDレコード
ord-0bfff4e7d8b442118e776fed1afb5023
出典データセット
uspto-grants-2003_05
特許番号
US06559312B2

反応ノート

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