Methyl iodide → 2-Bromo-3-methoxybenzaldehyde

HRID 563725ノート

反応式

HRID 563725 の反応式
[Br:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[C:11](=O)([O-])[O-].[K+].[K+].IC>O.CCOC(C)=O>[Br:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5]

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 37146742-Bromo-3-hydroxybenzaldehyde

生成物 1

HCID 118102632-Bromo-3-methoxybenzaldehyde

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-bromo-3-hydroxybenzaldehyde (0.5 g, 2.4 mmol) was added potassium carbonate (0.77 g, 5.6 mmol), and the mixture was stirred for 5 minutes. Iodomethane (0.17 mL, 2.7 mmol) was added, and the reaction was stirred at room temperature for 2 hours. The mixture was diluted with H2O (30 mL) and EtOAc (30 mL), and the organic layer was washed with 1N aqueous NaOH, then brine, dried over Na2SO4, decanted, and concentrated. The residue was purified by silica gel chromatography (0-60% EtOAc in hexanes) to give the title compound.

後処理

  1. stirringthe reaction was stirred at room temperature for 2 hours
  2. washthe organic layer was washed with 1N aqueous NaOH
  3. dry with materialbrine, dried over Na2SO4
  4. customdecanted
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel chromatography (0-60% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-a60dda44db3b4cb3938d0fbe610aa3c7
出典データセット
uspto-grants-2011_11
特許番号
US08067445B2

反応ノート

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