Methyl iodide → 2-Bromo-3-methoxybenzaldehyde

HRID 1810485노트

반응식

HRID 1810485 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 118102632-Bromo-3-methoxybenzaldehyde

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d85383ad4d284a1dafd7e6d8f454980a
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362044B2

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