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Hydrogen Peroxide → 3-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-benzyloxybenzoic Acid

HRID 1245158
ノート
印刷プレビュー

反応式

HRID 1245158 の反応式
[CH3:1][O:2][C:3]1[C:4]([CH3:32])=[C:5]([C:23]([O:30][CH3:31])=[C:24]([O:28][CH3:29])[C:25]=1[O:26][CH3:27])[CH2:6][C:7]1[C:8]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:9]([CH:12]=[CH:13][CH:14]=1)[CH:10]=[O:11].P([O-])(O)(O)=[O:34].[Na+].Cl[O-].[Na+].OO>C(#N)C.O>[CH3:1][O:2][C:3]1[C:4]([CH3:32])=[C:5]([C:23]([O:30][CH3:31])=[C:24]([O:28][CH3:29])[C:25]=1[O:26][CH3:27])[CH2:6][C:7]1[C:8]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:9]([CH:12]=[CH:13][CH:14]=1)[C:10]([OH:34])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 21919151HCID 21919151、化合物HCID 23665760Sodium HypochloriteHCID 23672064Monosodium phosphate

生成物 1

HCID 219192093-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-benzyloxybenzoic Acid収率 98.1%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6342Acetonitrile溶媒

実験手順

To a solution of 3-(3,4,5,6-tetramethoxy-2-methylbenzyl)-2-benzyloxybenzaldehyde (1.87 g, 4.28 mmol) in acetonitrile (12.0 ml) were added an aqueous solution (7.0 ml) of sodium dihydrogen phosphate (4.01 g, 33.42 mmol), an aqueous solution (7.0 ml) of sodium hypochlorite (1.74 g, 19.33 mmol) and an aqueous hydrogen peroxide (1.89 ml, 30%) and the mixture was stirred at room temperature for 5 hours. The reaction solution was diluted with water and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium hydrosulfite (Na2S2O4) and a saturated saline, dried and concentrated to give the title compound (1.90 g, 4.20 mmol, 98%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with a saturated aqueous solution of sodium hydrosulfite (Na2S2O4)
  3. customa saturated saline, dried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-fb6a4b37562045548124ac3df07fca59
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07122543B2

反応ノート

読み込み中…

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