1-Benzyl-4-(3,4-dimethoxyphenyl)piperidin-4-ol → 1-Benzyl-4-(3,4-dimethoxyphenyl)-1,2,3,6-tetrahydropyridine

HRID 1272278ノート

反応式

HRID 1272278 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=2)(O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C>[CH2:1]([N:8]1[CH2:9][CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=2)[CH2:12][CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

3

反応物 1

HCID 135355651-Benzyl-4-(3,4-dimethoxyphenyl)piperidin-4-ol

生成物 1

HCID 124107571-Benzyl-4-(3,4-dimethoxyphenyl)-1,2,3,6-tetrahydropyridine収率 90%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To acetic acid (130 ml) was added 1-benzyl-4-(3,4-dimethoxyphenyl)piperidine-4-ol (26.0 g, 79.4 mmol) obtained in Reference Example 14. The mixture was refluxed for 3 hours. The reaction mixture was concentrated, and the residue was made to basic with a solution of potassium carbonate and extracted with ethyl acetate. The organic extract was washed with water and saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residual crystals were washed with hexane to obtain 22.0 g (yield 90%) of the title compound. mp. 94–96° C.

後処理

  1. customobtained in Reference Example 14
  2. temperatureThe mixture was refluxed for 3 hours
  3. concentrationThe reaction mixture was concentrated
  4. extractionextracted with ethyl acetate
  5. extractionThe organic extract
  6. washwas washed with water and saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. washThe residual crystals were washed with hexane

出典と根拠

ORDレコード
ord-c0c782e88080432b82482549d7550d20
出典データセット
uspto-grants-2007_04
特許番号
US07208495B2

反応ノート

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