Acetic Anhydride → 1-Acetyl-4-benzoylpiperidine

HRID 926475

反応式

HRID 926475 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.C(N(CC)CC)C.[CH3:23][C:24](OC(C)=O)=[O:25]>ClCCl>[C:8]([CH:10]1[CH2:15][CH2:14][N:13]([C:24](=[O:25])[CH3:23])[CH2:12][CH2:11]1)(=[O:9])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 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) in dichloromethane (13.2 mL) and triethylamine (1.10 mL, 7.90 mmol) was treated with Ac2O (0.373 mL, 3.95 mmol) dropwise over 1 minute in 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 extracted with 1 M aqueous HCl (1×8 mL) and 1 M aqueous 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. extractionThe reaction was then extracted with 1 M aqueous HCl (1×8 mL) and 1 M aqueous 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-fa50c2a622f64a64a1a7a01dcbcfa1c7
出典データセット
uspto-grants-2016_03
特許番号
US09284308B2

関連ノート

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