Sodium Carbonate → 3,3-Dimethylcyclohexanone oxime

HRID 547668

反応式

HRID 547668 の反応式
[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][CH2:5][C:4](=O)[CH2:3]1.Cl.[NH2:11][OH:12].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.O>[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][CH2:5][C:4](=[N:11][OH:12])[CH2:3]1

参加物

6

実験手順

To a mixture of 3,3-dimethylcyclohexanone (4.0 g, 0.032 mol) and hydroxylamine hydrochloride (2.9 g, 0.041 mol) in ethanol (20 mL) was added dropwise a solution of sodium carbonate (4.3 g, 0.041 mol) in water (25 mL). The mixture was heated at reflux for 3 hours. The mixture was concentrated in vacuo to remove the ethanol and the aqueous residue was extracted with ethyl acetate. The organic phase was dried (MgSO4), filtered and concentrated in vacuo to give 3,3-dimethylcyclohexanone oxime as a yellow oil. This material was used without further purification.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 3 hours
  3. concentrationThe mixture was concentrated in vacuo
  4. customto remove the ethanol
  5. extractionthe aqueous residue was extracted with ethyl acetate
  6. dry with materialThe organic phase was dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bc52a2beb3c9464f9acefb0640c1fcc3
出典データセット
uspto-grants-2011_05
特許番号
US07939528B2

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