Acetic Anhydride → 1-Acetyl-4-benzoylpiperidine

HRID 627496

反応式

HRID 627496 の反応式
Cl.[C:2]1([C:8]([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:16][C:17](OC(C)=O)=[O:18]>C(Cl)Cl>[C:8]([CH:10]1[CH2:15][CH2:14][N:13]([C:17](=[O:18])[CH3:16])[CH2:12][CH2:11]1)(=[O:9])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 27244374-Benzoylpiperidine hydrochloride

生成物 1

HCID 27407141-Acetyl-4-benzoylpiperidine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of phenyl(piperidin-4-yl)methanone hydrochloride (743 mg, 3.29 mmol, Apollo Scientific) in DCM (13.2 mL) and TEA (1.10 mL, 7.90 mmol) was treated with Ac2O (0.373 mL, 3.95 mmol) dropwise over 1 min on an ice bath under argon, and the resulting translucent mixture was immediately removed from the ice bath and stirred at room temperature overnight. The reaction was then partitioned with 1 M HCl (1×8 mL) and 1 M NaOH (1×8 mL), and the organic layer was dried (Na2SO4), filtered, and concentrated to provide the title compound as a translucent beige oil that crystallized upon standing.

後処理

  1. customthe resulting translucent mixture was immediately removed from the ice bath
  2. customThe reaction was then partitioned with 1 M HCl (1×8 mL) and 1 M NaOH (1×8 mL)
  3. dry with materialthe organic layer was dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-7e76c6bd2a5040c4997c089712112ea1
出典データセット
uspto-grants-2016_04
特許番号
US09309222B2

関連ノート

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