Formaldehyde → 2-(1-Acetylpiperidin-4-yl)propenal

HRID 487474ノート

反応式

HRID 487474 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][OH:12])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl-].[CH3:14][NH2+]C.C=O>>[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([C:10](=[CH2:14])[CH:11]=[O:12])[CH2:8][CH2:9]1)(=[O:3])[CH3:2]

参加物

4

反応物 3

HCID 712FormaldehydeHCID 12954980Dimethylazanium;chlorideHCID 21468226Ethanone,1-[4-(2-hydroxyethyl)-1-piperidinyl]-

生成物 1

HCID 451192142-(1-Acetylpiperidin-4-yl)propenal

実験手順

3.95 g (23.3 mmol) of 2-(1-acetylpiperidin-4-yl)ethanol, 2.12 g (26.3 mmol) of dimethylammonium chloride and 3 ml (40 mmol) of 37% formaldehyde solution are heated at 110° C. for 2 hours with stirring. The mixture is allowed to cool and is extracted several times with diethyl ether. The organic phases are combined, washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated to dryness by evaporation. 2-(1-acetylpiperidin-4-yl)propenal is obtained in the form of a yellowish oil which can be further reacted without further purification.

後処理

  1. temperatureto cool
  2. extractionis extracted several times with diethyl ether
  3. washwashed with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness by evaporation

出典と根拠

ORDレコード
ord-604b3f2eec244a168750a5e227725d99
出典データセット
uspto-grants-1994_03
特許番号
US05294734

反応ノート

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