Methyl iodide → 3-Iodo-2-methoxybenzaldehyde

HRID 1486179ノート

反応式

HRID 1486179 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-ab3f82c431784536a66fce80973b04cc
出典データセット
uspto-grants-2016_08
特許番号
US09422314B2

反応ノート

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