Methyl iodide → 1-(2-Hydroxy-4-methoxy-phenyl)-2-methyl-propan-1-one

HRID 493188ノート

反応式

HRID 493188 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:13])[CH:10]([CH3:12])[CH3:11].IC.[C:16]([O-])([O-])=O.[Cs+].[Cs+]>C(#N)C>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:16])[CH:5]=[CH:4][C:3]=1[C:9](=[O:13])[CH:10]([CH3:11])[CH3:12]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 159157311-(2,4-Dihydroxyphenyl)-2-methylpropan-1-one

生成物 1

HCID 687238621-(2-Hydroxy-4-methoxy-phenyl)-2-methyl-propan-1-one

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The above prepared 1-(2,4-dihydroxy-phenyl)-2-methyl-propan-1-one (1.13 g, 5.55 mmol, corrected for purity) was dissolved in 22 mL of acetonitrile and treated successively at 0° C. with iodomethane (0.36 mL, 1.05 eq.) and Cs2CO3 (1.998 g, 1.1 eq.), and the mixture then stirred over night at ambient temperature. Pouring onto crashed ice/NH4Cl, twofold extraction with AcOEt, washing with water, drying over sodium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=95/5), delivered 0.740 g of the title compound as colorless oil.

後処理

  1. additionPouring
  2. extractionice/NH4Cl, twofold extraction with AcOEt
  3. washwashing with water
  4. dry with materialdrying over sodium sulfate, and evaporation of the solvents

出典と根拠

ORDレコード
ord-7e46fa0d283c44ef827412d5e7d16e22
出典データセット
uspto-grants-2009_05
特許番号
US07534788B2

反応ノート

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