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

HRID 222185

반응식

HRID 222185 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 866142543,3-Dimethylindan-1-one oxime수율 97.4%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-802a245a9a154b8a85e7196884e91751
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207177B2

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