Methyl iodide → 2-Hydroxy-4-methoxybenzophenone

HRID 493196

反応式

HRID 493196 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:10].[C:17]([O-])([O-])=O.[Cs+].[Cs+].IC>C(#N)C>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:17])[CH:5]=[CH:4][C:3]=1[C:9]([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)=[O:10]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 85722,4-DihydroxybenzophenoneHCID 10796Cesium carbonate

生成物 1

HCID 46322-Hydroxy-4-methoxybenzophenone

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The above prepared (2,4-dihydroxy-phenyl)-phenyl-methanone (0.775 g, 3.62 mmol) was dissolved in 15 mL of acetonitrile and treated successively at 0° C. with Cs2CO3 (1.297 g, 1.1 eq.) and iodomethane (0.242 mL, 1.08 eq.), and the mixture was 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, heptane/AcOEt=9/1), delivered 0.681 g of the title compound as off-white 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-c7f63306a63f49d0aaaa50c748b9e9e7
出典データセット
uspto-grants-2009_05
特許番号
US07534788B2

関連ノート

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