Diethyl Ether → 4-Acetylpiperidin-2-one

HRID 535313노트

반응식

HRID 535313 반응식
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]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 86718437N-methoxy-N-methyl-2-oxopiperidine-4-carboxamideHCID 178418689HCID 178418689, 화합물

생성물 1

HCID 571689834-Acetylpiperidin-2-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3896b49d54cc4dc2b9c435c680afe2c3
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859535B2

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