Hydrogen Peroxide → 1-(4-Hydroxyphenoxy)-2-(3-Methoxyphenyl)-6-Methoxynaphthalene

HRID 2213164ノート

反応式

HRID 2213164 の反応式
C([C:3]1[CH:29]=[CH:28][C:6]([O:7][C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=3)[CH:11]=[CH:10][C:9]=2[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([O:26][CH3:27])[CH:21]=2)=[CH:5][CH:4]=1)=O.OO.[OH:32]S(O)(=O)=O.C([O-])(O)=O.[Na+]>CO>[OH:32][C:3]1[CH:29]=[CH:28][C:6]([O:7][C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=3)[CH:11]=[CH:10][C:9]=2[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([O:26][CH3:27])[CH:21]=2)=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 120741741-(4-Formylphenoxy)-2-(3-Methoxyphenyl)-6-Methoxynaphthalene

生成物 1

HCID 120741751-(4-Hydroxyphenoxy)-2-(3-Methoxyphenyl)-6-Methoxynaphthalene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

2.3 g (6 mmol) of 1-(4-formylphenoxy)-2-(3-methoxyphenyl)-6-methoxynaphthalene was suspended in 15 mL of MeOH and 1.7 mL (9 mmol) of 30% H2O2 was added. To the stirring mixture, 0.76 mL of conc. H2SO4 was slowly added. An additional 30 mL of MeOH was added and the reaction was allowed to proceed for forty-eight hours. The reaction was neutralized with NaHCO3 solution and extracted with CHCl3. The CHCl3 was washed with brine, dried with Na2SO4, and chromatographed on a silica gel column eluted with CHCl3. This yielded 1.6 g of the title compound as a tan amorphous powder, mp 125–126° C.

後処理

  1. waitto proceed for forty-eight hours
  2. extractionextracted with CHCl3
  3. washThe CHCl3 was washed with brine
  4. dry with materialdried with Na2SO4
  5. customchromatographed on a silica gel column
  6. washeluted with CHCl3

出典と根拠

ORDレコード
ord-90ead16527d74fa7af0c246243e4cf15
出典データセット
uspto-grants-2006_09
特許番号
US07105541B2

反応ノート

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