Phenol → HCID 18347201、化合物

HRID 2269565ノート

反応式

HRID 2269565 の反応式
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([S:18][CH3:19])=[CH:14][CH:13]=1)=[O:11].C([O-])([O-])=O.[K+].[K+]>CC(C)=O.CCCCCC.CCOC(C)=O>[O:7]([CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([S:18][CH3:19])=[CH:14][CH:13]=1)=[O:11])[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 3

HCID 996PhenolHCID 11430Potassium CarbonateHCID 27375232-Bromo-1-(4-methylsulfanylphenyl)ethanone

生成物 1

HCID 18347201HCID 18347201、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 21226206Ethyl acetate hexane溶媒

実験手順

To a solution of phenol (9.4 g) and 2-bromo-1-(4-(methylthio)phenyl)ethanone (12.5 g) in 500 mL of acetone was added K2CO3 (13.8 g). The mixture was refluxed for 12 h, then diluted with 500 mL of 1:1 hexane/EtOAc. The solid was removed by filtration and the filtrate was concentrated. The residue was dissolved in Et2O (500 mL), washed with 1N NaOH (100 ml) and dried over MgSO4. After filtration and concentration, the title compound (9 g) was collected by filtration and air dried.

後処理

  1. temperatureThe mixture was refluxed for 12 h
  2. customThe solid was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was dissolved in Et2O (500 mL)
  5. washwashed with 1N NaOH (100 ml)
  6. dry with materialdried over MgSO4
  7. filtrationAfter filtration and concentration
  8. filtrationthe title compound (9 g) was collected by filtration and air
  9. customdried

出典と根拠

ORDレコード
ord-751651874417468293329595a7611527
出典データセット
uspto-grants-2001_12
特許番号
US06329421B1

反応ノート

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