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Methyl iodide → 1-(2-Amino-3-methoxyphenyl)ethan-1-one

HRID 1710815
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HRID 1710815 반응식
CI.[C:3](=O)([O-])[O-].[K+].[K+].[NH2:9][C:10]1[C:15]([OH:16])=[CH:14][CH:13]=[CH:12][C:11]=1[C:17](=[O:19])[CH3:18]>CN(C=O)C>[NH2:9][C:10]1[C:15]([O:16][CH3:3])=[CH:14][CH:13]=[CH:12][C:11]=1[C:17](=[O:19])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 205912'-Amino-3'-hydroxyacetophenone

생성물 1

HCID 136911411-(2-Amino-3-methoxyphenyl)ethan-1-one수율 96.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Under an atmosphere of nitrogen, methyl iodide (1.35 g, 10 mmol) and potassium carbonate (4.39 g, 320 mmol) were added to a solution of 2′-amino-3′-hydroxyacetophenone (960 mg, 6 mmol, TCI Europe) in DMF (6 ml). The reaction mixture was stirred for 1 h at r.t., during which time the color of the mixture changed from light brown to dark green. The mixture was then worked up by extraction with H2O/ethyl acetate, drying of the organic phase (Na2SO4), and evaporation of solvent. The title compound (960 mg, 92%) was isolated from the residue by column chromatography (silica gel, heptan/ethyl acetate=100/0-70/30).

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후처리

  1. extractionThe mixture was then worked up by extraction with H2O/ethyl acetate
  2. dry with materialdrying of the organic phase (Na2SO4), and evaporation of solvent

출처 및 근거

ORD 기록
ord-0b0278f1ce8b4866908d04d138df1280
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790733B2

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