Hydrogen Peroxide → HCID 10867638、化合物

HRID 1422317ノート

反応式

HRID 1422317 の反応式
[CH2:1]([O:8][C:9]1[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][C:10]=1C=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(=O)(=O)(O)[OH:19].OO>CO>[CH2:1]([O:8][C:9]1[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][C:10]=1[OH:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 110641372-benzyloxy-3-methylbenzaldehyde

生成物 1

HCID 10867638HCID 10867638、化合物収率 70%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-Benzyloxy-3-methylbenzaldehyde prepared by the above 2-(1) 20.0 g (88.4 mmol) was dissolved in methanol 100 ml and thereto was added sulfuric acid 20.0 g (203 mmol) and then added 30% hydrogen peroxide 30.1 g (265 mmol). The mixture was refluxed for 2 hours. After disappearance of the raw material, the solution was concentrated in vacuo, neutralized with a saturated sodium bicarbonate solution and extracted with methylene chloride. The solvent was removed in vacuo and the residue was purified by silica gel chromatography (n-hexane-ethyl acetate) to give 2-benzyloxy-3-methylphenol 13.3 g (yield: 70%).

後処理

  1. temperatureThe mixture was refluxed for 2 hours
  2. concentrationAfter disappearance of the raw material, the solution was concentrated in vacuo
  3. extractionextracted with methylene chloride
  4. customThe solvent was removed in vacuo
  5. customthe residue was purified by silica gel chromatography (n-hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-6a2446198f034f78870c6c4abbe55acc
出典データセット
uspto-grants-2000_06
特許番号
US06080895

反応ノート

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