3-Methoxyphenol → 1-(3-Methoxyphenoxy)-4,4-dimethyl-2-pentanone

HRID 2185055ノート

反応式

HRID 2185055 の反応式
Br[CH2:2][C:3](=[O:9])[CH2:4][C:5]([CH3:8])([CH3:7])[CH3:6].[CH3:10][O:11][C:12]1[CH:13]=[C:14]([OH:18])[CH:15]=[CH:16][CH:17]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH:15]=[CH:16][CH:17]=1)[O:18][CH2:2][C:3](=[O:9])[CH2:4][C:5]([CH3:8])([CH3:7])[CH3:6]

参加物

5

反応物 3

HCID 90073-MethoxyphenolHCID 10796Cesium carbonateHCID 2225851-Bromo-4,4-dimethylpentan-2-one

生成物 1

HCID 224590191-(3-Methoxyphenoxy)-4,4-dimethyl-2-pentanone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A stirred solution of the product from Step B (1.626 grams) in dry DMF (18 mL) was combined with 3-methoxyphenol (1.256 grams) and cesium carbonate (3.292 grams). The mixture was stirred for 2.5 hours. The reaction was partitioned between isopropyl acetate and pH4 pthalate buffer. The organic was washed twice with water, dried over magnesium sulfate and filtered. Concentration furnished an oil from which the title compound was isolated by chromatography over silica gel (4:1 hex/ethyl acetate).

後処理

  1. customThe reaction was partitioned between isopropyl acetate and pH4
  2. washThe organic was washed twice with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationConcentration

出典と根拠

ORDレコード
ord-353fa67eaf91444884bdc6f3ff8ec5ae
出典データセット
uspto-grants-2002_06
特許番号
US06399640B1

反応ノート

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