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

HRID 622679ノート

反応式

HRID 622679 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-de99814f1c6945d2932bb6a066032068
出典データセット
uspto-grants-1988_09
特許番号
US04772618

反応ノート

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