Benzaldehyde, 4-(phenylmethoxy)- → 4-Benzyloxy-benzaldehyde oxime

HRID 77737

反応式

HRID 77737 の反応式
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:17][OH:18].Cl.C([O-])(=O)C.[Na+]>C(O)C.O>[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[N:17][OH:18])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 78109Benzaldehyde, 4-(phenylmethoxy)-HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium Acetate

生成物 1

HCID 7633594-Benzyloxy-benzaldehyde oxime

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒2 回

実験手順

4.24 g of 4-benzyloxy benzaldehyde (20 mmol) was dissolved in a 0.2M mixed solution of ethanol and water (3:1,100 ml), followed by stirring. 2.78 g of NH2OH—HCl (40 mmol) and 2.46 g of sodium acetate(30 mmol) were added thereto, and stirred at room temperature for about 30 minutes. Subsequently, the completion of the reaction was confirmed by liquid chromatography, and water and ethanol were removed by distillation under reduced pressure to obtain a pale yellow solid compound. The pale yellow solid compound was extracted three times with water and ethyl acetate, an organic solvent layer was dried under reduced pressure to obtain a crude product, and the crude product was then purified with a hexane/ethylacetate solution (10:1) to obtain a white solid compound. The obtained solid compound was subjected to subsequent reactions without additional purification.

後処理

  1. stirringstirred at room temperature for about 30 minutes
  2. customwere removed by distillation under reduced pressure
  3. customto obtain a pale yellow solid compound
  4. extractionThe pale yellow solid compound was extracted three times with water and ethyl acetate
  5. customan organic solvent layer was dried under reduced pressure

出典と根拠

ORDレコード
ord-3f0ce4815c904f29a068b340a3954c8a
出典データセット
uspto-grants-2014_09
特許番号
US08841335B2

関連ノート

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