1-Phenyl-4-piperidinone → 1-Phenyl-piperidin-4-one oxime

HRID 37849

反応式

HRID 37849 の反応式
[C:1]1([N:7]2[CH2:12][CH2:11][C:10](=O)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[NH2:15][OH:16]>CO>[C:1]1([N:7]2[CH2:12][CH2:11][C:10](=[N:15][OH:16])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 4130091-Phenyl-4-piperidinoneHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 3438331-Phenyl-piperidin-4-one oxime収率 92%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 1-phenyl-piperidin-4-one (180 mg, 1.03 mmol) and hydroxylamine hydrochloride (142 mg, 2.06 mmol) in methanol (10 mL) was heated at reflux for 6 h. The solvent was evaporated and the residue diluted with water. The mixture was extracted with ethyl acetate then the organic phase was washed with water, brine, dried over anhydrous sodium sulfate and concentrated to afford 1-phenyl-piperidin-4-one oxime (0.18 g, 92%) as a liquid.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 6 h
  3. customThe solvent was evaporated
  4. additionthe residue diluted with water
  5. extractionThe mixture was extracted with ethyl acetate
  6. washthe organic phase was washed with water, brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-1a67ca0e59ef49e293898d43ff28ca5e
出典データセット
uspto-grants-2013_09
特許番号
US08524705B2

関連ノート

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