Piperidine → Piperidine, 1-(4-nitrophenyl)-

HRID 1079392ノート

反応式

HRID 1079392 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[NH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1>CN(C)C=O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:3][CH:4]=1)([O-:10])=[O:9]

参加物

4

実験手順

A solution of p-fluoronitrobenzene (31.8 ml) in dimethylformamide (200 ml) was ice-cooled and to this was added piperidine (60 ml) dropwise, followed by stirring with ice cooling for 2 hours. After the solvent was distilled off, the residual oily product was dissolved in ethyl acetate ester (200 ml), followed by washing in turn with aqueous saturated solution of sodium bicarbonate and water. Then, the solution was dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was recrystallized from n-hexane to obtain N-(4-nitrophenyl)piperidine as yellow crystals (52.8 g).

後処理

  1. temperaturecooled
  2. distillationAfter the solvent was distilled off
  3. dissolutionthe residual oily product was dissolved in ethyl acetate ester (200 ml)
  4. washby washing in turn with aqueous saturated solution of sodium bicarbonate and water
  5. dry with materialThen, the solution was dried over anhydrous magnesium sulfate
  6. distillationAfter the solvent was distilled off
  7. customthe residue was recrystallized from n-hexane

出典と根拠

ORDレコード
ord-2cf7a327371f4730a5c5bfa29490dc36
出典データセット
uspto-grants-1996_12
特許番号
US05580883

反応ノート

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