Methanol → Methyl 4-(piperidin-4-yl)benzoate

HRID 478640노트

반응식

HRID 478640 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([C:7]2[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.[CH3:16]O>>[CH3:16][O:12][C:11](=[O:13])[C:10]1[CH:14]=[CH:15][C:7]([CH:4]2[CH2:5][CH2:6][NH:1][CH2:2][CH2:3]2)=[CH:8][CH:9]=1

참가 물질

3

반응물 2

HCID 887MethanolHCID 180024624-(Piperidin-4-yl)benzoic acid

생성물 1

HCID 24904226Methyl 4-(piperidin-4-yl)benzoate

실험 절차

4-Piperidin-4-yl-benzoic acid (47 mmol) is dissolved in methanol (300 ml) and 1 ml of concentrated sulfonic acid is added. The mixture is heated under reflux overnight. After evaporation of the solvent, the residue is dissolved in a mixture of water and sodium carbonate (to ensure basic conditions) and extracted three times with ethyl acetate. The combined extract is dried over sodium sulfate and evaporated. A brown powder with Rf=0.18 (CH2Cl2/MeOH=9:1) is obtained.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux overnight
  3. customAfter evaporation of the solvent
  4. dissolutionthe residue is dissolved in a mixture of water and sodium carbonate (to ensure basic conditions)
  5. extractionextracted three times with ethyl acetate
  6. extractionThe combined extract
  7. dry with materialis dried over sodium sulfate
  8. customevaporated
  9. customA brown powder with Rf=0.18 (CH2Cl2/MeOH=9:1) is obtained

출처 및 근거

ORD 기록
ord-10bb8a05683e45f7a5dd016b41686167
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06642239B2

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