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

HRID 253454

반응식

HRID 253454 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-3c53600ed01e4328b9b0ac80bc165aa0
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07872018B2

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