Diethyl Ether → 4-Acetylpiperidin-2-one

HRID 535313ノート

反応式

HRID 535313 の反応式
CON(C)[C:4]([CH:6]1[CH2:11][CH2:10][NH:9][C:8](=[O:12])[CH2:7]1)=[O:5].C[Mg+].[Br-].[CH3:17]COCC>C1COCC1>[C:4]([CH:6]1[CH2:11][CH2:10][NH:9][C:8](=[O:12])[CH2:7]1)(=[O:5])[CH3:17]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 86718437N-methoxy-N-methyl-2-oxopiperidine-4-carboxamideHCID 178418689HCID 178418689、化合物

生成物 1

HCID 571689834-Acetylpiperidin-2-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of N-methoxy-N-methyl-2-oxopiperidine-4-carboxamide (2.72 g, 9.79 mmol) in THF (30 ml) was immersed in an ice-bath. MeMgBr (3M) in Et2O (4.57 ml, 13.70 mmol) was added slowly and the remaining white suspension was stirred for 1 h in an ice-bath and over night at room temperature. The reaction mixture was quenched carefully with aqueous saturated NaHCO3 and extracted with DCM. The organic layers were washed with brine, combined, dried over Na2SO4, filtered and concentrated in vacuo to obtain the title compound as yellow-brown oil. The crude product was directly used in the next step.

後処理

  1. customThe reaction mixture was quenched carefully with aqueous saturated NaHCO3
  2. extractionextracted with DCM
  3. washThe organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3896b49d54cc4dc2b9c435c680afe2c3
出典データセット
uspto-grants-2014_10
特許番号
US08859535B2

反応ノート

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