4'-Hydroxypropiophenone → HCID 86085445、化合物

HRID 1669247

反応式

HRID 1669247 の反応式
[OH-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:13])[CH2:11][CH3:12])=[CH:6][CH:5]=1.Cl[CH2:15][C:16]1[C:17]([CH3:25])=[C:18]([CH3:24])[CH:19]=[C:20]([CH3:23])[C:21]=1[CH3:22]>CCO.O>[CH3:22][C:21]1[C:20]([CH3:23])=[CH:19][C:18]([CH3:24])=[C:17]([CH3:25])[C:16]=1[CH2:15][O:3][C:4]1[CH:5]=[CH:6][C:7]([C:10](=[O:13])[CH2:11][CH3:12])=[CH:8][CH:9]=1

参加物

6

反応物 3

HCID 62714'-HydroxypropiophenoneHCID 14798Sodium HydroxideHCID 819393-(Chloromethyl)-1,2,4,5-tetramethylbenzene

生成物 1

HCID 86085445HCID 86085445、化合物収率 67.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

NaOH (1.6 g, 40 mmol) is added to the solution of 1-(4-hydroxy-phenyl)-propan-1-one (3.0 g, 20 mmol) in EtOH (50 mL) and water (30 mL), followed by the addition of 3-Chloromethyl-1,2,4,5-tetramethyl-benzene (5.5 g, 30 mol). The resulting mixture is heated to turn into clear solution and stirred at room temperature overnight. The reaction is quenched by 1N HCl and extracted with ethyl acetate (3×100 mL). The combined organic layers are washed with water, brine, dried (MgSO4), concentrated and chromatographed to afford the titled compound as a white solid (4.0 g).

後処理

  1. temperatureThe resulting mixture is heated
  2. customThe reaction is quenched by 1N HCl
  3. extractionextracted with ethyl acetate (3×100 mL)
  4. washThe combined organic layers are washed with water, brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customchromatographed

出典と根拠

ORDレコード
ord-c3a58e85ffe24f79bd6fe328aa87a9f6
出典データセット
uspto-grants-2011_08
特許番号
US07989457B2

関連ノート

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