Dichloromethane → 2-Chloro-4-hydroxy-5-methoxybenzaldehyde

HRID 253454

反応式

HRID 253454 の反応式
[Cl:1][C:2]1[CH:9]=[C:8]([O:10]C)[C:7]([O:12][CH3:13])=[CH:6][C:3]=1[CH:4]=[O:5].ClCCl.[Cl-].[Cl-].[Cl-].[Al+3]>O>[Cl:1][C:2]1[CH:9]=[C:8]([OH:10])[C:7]([O:12][CH3:13])=[CH:6][C:3]=1[CH:4]=[O:5]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 2793512-Chloro-4,5-dimethoxybenzaldehydeHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 290002-Chloro-4-hydroxy-5-methoxybenzaldehyde

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Chloro-4,5-dimethoxy-benzaldehyde (135, 2.00 g, 0.00997 mol), dichloromethane (73.44 mL) and aluminum trichloride (2.50 g, 0.0187 mol) were combined under an atmosphere of nitrogen. The reaction was stirred at room temperature overnight. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and washed with 5% ethyl acetate in hexane to provide an off-white solid (136, 757 mg, 41%). MS (ESI) [M−H+]−=185.0, 187.0.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. washwashed with 5% ethyl acetate in hexane
  6. customto provide an off-white solid (136, 757 mg, 41%)

出典と根拠

ORDレコード
ord-3c53600ed01e4328b9b0ac80bc165aa0
出典データセット
uspto-grants-2011_01
特許番号
US07872018B2

関連ノート

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