Ammonium Acetate → 2,4-Dimethyl-4,5-dihydro[3,4'-bipyridin]-6(1H)-one

HRID 1388309노트

반응식

HRID 1388309 반응식
[C:1]([CH:4]([C:13]1[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=1)[CH:5]([CH3:12])[CH2:6][C:7](OCC)=[O:8])(=O)[CH3:2].C([O-])(=O)C.[NH4+:23]>C(O)C>[CH3:12][CH:5]1[C:4]([C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[C:1]([CH3:2])[NH:23][C:7](=[O:8])[CH2:6]1

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 20470813Ethyl 4-Acetyl-3-methyl-4-(4-pyridinyl)butanoate

생성물 1

HCID 132689722,4-Dimethyl-4,5-dihydro[3,4'-bipyridin]-6(1H)-one수율 9.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture containing 24 g of ethyl 4-acetyl-3-methyl-4-(4-pyridinyl)butanoate, 7 g of ammonium acetate and 50 ml of ethanol was refluxed for 8 hours with stirring. The reaction mixture was then concentrated to dryness in vacuo and the remaining white solid was collected, washed with ethanol and dried to produce 1.8 g of 3,4-dihydro-4,6-dimethyl-5-(4-pyridinyl)-2(1H)-pyridinone, m.p. 184°-185° C. It's nmr and mass spectrum were consistent with the assigned structure.

후처리

  1. temperaturewas refluxed for 8 hours
  2. concentrationThe reaction mixture was then concentrated to dryness in vacuo
  3. customthe remaining white solid was collected
  4. washwashed with ethanol
  5. customdried

출처 및 근거

ORD 기록
ord-fecc8dc1a9f7440194bba5f05fb379e7
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431651

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