Water → Cyclohexanone, 2-(3-methoxyphenyl)-, oxime

HRID 1594919ノート

反応式

HRID 1594919 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]2=O)[CH:6]=[CH:7][CH:8]=1.Cl.[NH2:17][OH:18].C([O-])(=O)C.[Na+].O>CCO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]2=[N:17][OH:18])[CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 962WaterHCID 858682-(3-Methoxyphenyl)cyclohexanoneHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium Acetate

生成物 1

HCID 2728109Cyclohexanone, 2-(3-methoxyphenyl)-, oxime

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-(3-Methoxyphenyl)-cyclohexanone, as described in Step A above, (0.61 g, 3 mmol), hydroxylamine hydrochloride (0.40 g, 6 mmol) and sodium acetate (0.80, 6.2 mmol) were combined in EtOH (4 mL): H2O (2 mL) and heated at reflux for 3 h. The reaction mixture was concentrated, then partitioned between EtOAc (100 mL) and H2O (100 mL), the organic layer separated, washed with H2O, brine, and dried (MgSO4). Filtration and concentration to dryness gave the title compound.

後処理

  1. temperatureat reflux for 3 h
  2. concentrationThe reaction mixture was concentrated
  3. custompartitioned between EtOAc (100 mL) and H2O (100 mL)
  4. customthe organic layer separated
  5. washwashed with H2O, brine
  6. dry with materialdried (MgSO4)
  7. filtrationFiltration and concentration to dryness

出典と根拠

ORDレコード
ord-0723351be00e4feaab4906a065b4772b
出典データセット
uspto-grants-2001_09
特許番号
US06284755B1

反応ノート

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