Potassium Carbonate → 1-(2-Tetrahydrofurylmethyl)piperid-4-one oxime

HRID 622679노트

반응식

HRID 622679 반응식
[NH:1]1[CH2:6][CH2:5][C:4](=[N:7][OH:8])[CH2:3][CH2:2]1.CS(O[CH2:14][CH:15]1[CH2:19][CH2:18][CH2:17][O:16]1)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C(C)C>[O:16]1[CH2:17][CH2:18][CH2:19][CH:15]1[CH2:14][N:1]1[CH2:6][CH2:5][C:4](=[N:7][OH:8])[CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 266119(Tetrahydrofuran-2-yl)methyl methanesulfonateHCID 12849639N-Piperidin-4-ylidenehydroxylamine

생성물 1

HCID 212915121-(2-Tetrahydrofurylmethyl)piperid-4-one oxime수율 535.9%

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of piperid-4-one oxime (46 g; 0.04 moles), 2-tetrahydrofurylmethyl methanesulphonate (79.3 g; 0.44 moles) and anhydrous potassium carbonate (56.5 g; 0.40 moles) in methyl isobutyl ketone (625 ml), was boiled under reflux with stirring for 48 hours. After cooling, the reaction mixture was washed with brine, dried (Na2SO4), and the solvent removed in vacuo. The residue was crystallised from diisopropyl ether to give 1-(2-tetrahydrofurylmethyl)-piperid-4-one oxime (42.5 g), m.p. 104°-106°.

후처리

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. washthe reaction mixture was washed with brine
  4. dry with materialdried (Na2SO4)
  5. customthe solvent removed in vacuo
  6. customThe residue was crystallised from diisopropyl ether

출처 및 근거

ORD 기록
ord-de99814f1c6945d2932bb6a066032068
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772618

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