Ethanol → 2-(3-Pyridyl)-6-(4-pyridyl)pyrimidin-4-one

HRID 853786

반응식

HRID 853786 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7](=O)[CH2:8][C:9]([O:11]CC)=O)=[CH:3][CH:2]=1.Cl.[C:16]([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)(=[NH:18])[NH2:17].C(=O)([O-])[O-].[K+].[K+].C(O)C>C(O)(=O)C>[N:21]1[CH:22]=[CH:23][CH:24]=[C:19]([C:16]2[NH:18][C:9](=[O:11])[CH:8]=[C:7]([C:4]3[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=3)[N:17]=2)[CH:20]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 202042Nicotinamidine hydrochlorideHCID 2735202Ethyl 3-(4-pyridyl)-3-oxopropionate

생성물 1

HCID 1354093932-(3-Pyridyl)-6-(4-pyridyl)pyrimidin-4-one수율 50.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
75 °C

실험 절차

ethyl 3-(4-pyridyl)-3-oxopropionate (0.60 g), 3-amidinopyridine hydrochloride (0.54 g) and potassium carbonate (1.15 g) were added to 5 ml of ethanol, and the mixture was heated under reflux at 75° C. for 20 hours. Acetic acid was added to the reaction mixture, and the solvent was removed by distillation. The residue was added with water and then with acetic acid, and the resulting solid was separated by filtration, washed with water and ethyl acetate, and dried to obtain 0.39 g of the desired compound.

후처리

  1. temperaturethe mixture was heated
  2. customthe solvent was removed by distillation
  3. additionThe residue was added with water
  4. customwith acetic acid, and the resulting solid was separated by filtration
  5. washwashed with water and ethyl acetate
  6. customdried

출처 및 근거

ORD 기록
ord-80f553bfe6ea4338b734b2fe6562c22a
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07256199B1

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