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Dimethylamine → 1-Acetyl-3-(4-dimethylaminobenzoyl)piperidine

HRID 487160
ノート
印刷プレビュー

反応式

HRID 487160 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][CH2:7][CH:6]([C:10](=[O:18])[C:11]2[CH:16]=[CH:15][C:14](F)=[CH:13][CH:12]=2)[CH2:5]1)(=[O:3])[CH3:2].[CH3:19][NH:20][CH3:21].C(=O)([O-])O.[Na+]>>[C:1]([N:4]1[CH2:9][CH2:8][CH2:7][CH:6]([C:10](=[O:18])[C:11]2[CH:16]=[CH:15][C:14]([N:20]([CH3:21])[CH3:19])=[CH:13][CH:12]=2)[CH2:5]1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 674DimethylamineHCID 516892Sodium BicarbonateHCID 219398131-Acetyl-3-(4-fluorobenzoyl)piperidine

生成物 1

HCID 193908491-Acetyl-3-(4-dimethylaminobenzoyl)piperidine

実験手順

A mixture consisting of 2.49 g of 1-acetyl-3-(4-fluorobenzoyl)piperidine and 8 ml of 50% aqueous dimethylamine solution was stirred for 5 days at room temperature, followed by addition of a saturated aqueous solution of sodium hydrogen carbonate. The solution was extracted with ethyl acetate and the extract was dried. The solvent was then distilled off and the remaining oil was purified by silica gel column chromatography (eluent: ethyl acetate) to give 2.6 g of 1-acetyl-3-(4-dimethylaminobenzoyl)piperidine as a pale yellow oil.

後処理

  • extractionThe solution was extracted with ethyl acetate
  • customthe extract was dried
  • distillationThe solvent was then distilled off
  • customthe remaining oil was purified by silica gel column chromatography (eluent: ethyl acetate)
  • 出典と根拠

    ORDレコード
    ord-3a3b344894124513a4cbf9bcc41cc552
    出典データセット
    uspto-grants-1994_03
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US05294625

    反応ノート

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