Methyl iodide → 3-Iodo-2-methoxybenzaldehyde

HRID 1404366노트

반응식

HRID 1404366 반응식
[I:1][C:2]1[C:3]([OH:10])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[C:11](=O)([O-])[O-].[Cs+].[Cs+].CI>CC(N(C)C)=O.CCOCC>[I:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 152099202-Hydroxy-3-iodobenzaldehyde

생성물 1

HCID 108014193-Iodo-2-methoxybenzaldehyde

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 31374Dimethylacetamide용매

실험 절차

To a solution of 3-iodo-2-hydroxy-benzaldehyde (4.0 g, 16.06 mmol) in DMA (32 mL) was added cesium carbonate (5.85 g, 18 mmol) followed by methyl iodide (1.12 mL, 18 mmol). The resulting mixture was stirred for 4.75 hours then diluted with ether, washed with water, dried over magnesium sulfate and concentrated. The residue was purified by silica chromatography (50 g silica; eluted with 0-20% ethyl acetate in hexanes) to give the title compound as an oil.

후처리

  1. washwashed with water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by silica chromatography (50 g silica; eluted with 0-20% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-cae7c0572d9d4347ac38b10b26c20233
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08912169B2

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