Sodium Carbonate → 3,3-Dimethylcyclohexanone oxime

HRID 547668노트

반응식

HRID 547668 반응식
[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

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 76322Cyclohexanone, 3,3-dimethyl-HCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 594582653,3-Dimethylcyclohexanone oxime

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bc52a2beb3c9464f9acefb0640c1fcc3
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939528B2

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