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

HRID 853786

反応式

HRID 853786 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-80f553bfe6ea4338b734b2fe6562c22a
出典データセット
uspto-grants-2007_08
特許番号
US07256199B1

関連ノート

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