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

HRID 345444

反応式

HRID 345444 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31260Isoamyl Alcohol溶媒

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-b02f55d19ab9497a92240296f4862dc8
出典データセット
uspto-grants-1991_10
特許番号
US05057528

関連ノート

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