Sodium Hydroxide → 3,3-Dimethylindan-1-one oxime

HRID 222185

反応式

HRID 222185 の反応式
[CH3:1][C:2]1([CH3:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=O)[CH2:3]1.Cl.[NH2:14][OH:15].[OH-].[Na+]>CO.O>[CH3:1][C:2]1([CH3:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[N:14][OH:15])[CH2:3]1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 3046283,3-Dimethyl-1-indanoneHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 866142543,3-Dimethylindan-1-one oxime収率 97.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a solution of 3,3-dimethylindan-1-one (1.16 g, 7.21 mmol) and hydroxylamine hydrochloride (1.31 g, 18.8 mmol) in MeOH (20.0 mL) was added a solution of sodium hydroxide (765 mg, 19.1 mmol) in water (10.0 mL). The mixture was heated to 80° C. for 2 h. The cooled reaction was concentrated in vacuo and partitioned between DCM and water. The organic layer was separated and concentrated in vacuo to afford the title compound as an oil (1.23 g, 97%). LC/MS: Rt=1.61 min, ES+ 176 (AA standard).

後処理

  1. customThe cooled reaction
  2. concentrationwas concentrated in vacuo
  3. custompartitioned between DCM and water
  4. customThe organic layer was separated
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-802a245a9a154b8a85e7196884e91751
出典データセット
uspto-grants-2012_06
特許番号
US08207177B2

関連ノート

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