Piperidin-4-ol → 1-(Pyridin-4-yl)piperidin-4-ol

HRID 345444

반응식

HRID 345444 반응식
Cl.Cl[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.[OH:9][CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.C(=O)(O)[O-].[Na+]>C(O)CC(C)C>[N:6]1[CH:7]=[CH:8][C:3]([N:13]2[CH2:14][CH2:15][CH:10]([OH:9])[CH2:11][CH2:12]2)=[CH:4][CH:5]=1

참가 물질

5

반응물 3

HCID 79341Piperidin-4-olHCID 818524-Chloropyridine hydrochlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 234476191-(Pyridin-4-yl)piperidin-4-ol

시약·촉매·용매 1

HCID 31260Isoamyl Alcohol용매

실험 절차

A mixture of 4-chloropyridine hydrochloride (7.50 g), 4-hydroxypiperidine (5.06 g) and sodium bicarbonate (10.1 g) in isoamyl alcohol (60 ml) was heated under reflux with stirring for 60 hours and then evaporated. The residue was extracted several times with a boiling mixture of ethyl acetate/methanol (10:1) and the combined extracts were filtered and evaporated. The residue was sublimed at 120°-150° and 0.2 mm pressure to give the pure product, (7.30 g), m.p. 155°-156°.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux
  3. customevaporated
  4. extractionThe residue was extracted several times
  5. additionwith a boiling mixture of ethyl acetate/methanol (10:1)
  6. filtrationthe combined extracts were filtered
  7. customevaporated
  8. customwas sublimed at 120°-150°
  9. custom0.2 mm pressure to give the pure product, (7.30 g), m.p. 155°-156°

출처 및 근거

ORD 기록
ord-b02f55d19ab9497a92240296f4862dc8
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057528

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