Methyl iodide → 3-Iodo-2-methoxybenzaldehyde

HRID 1404366ノート

反応式

HRID 1404366 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 108014193-Iodo-2-methoxybenzaldehyde

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 31374Dimethylacetamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-cae7c0572d9d4347ac38b10b26c20233
出典データセット
uspto-grants-2014_12
特許番号
US08912169B2

反応ノート

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