Potassium Carbonate → N'-(6-Oxo-1,6-dihydropyridin-2-yl)-N,N-dipropylformimidamide

HRID 1607087ノート

反応式

HRID 1607087 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH:8][CH:9]=[N:10][CH2:11][CH2:12][CH3:13])[N:3]=1.[CH2:14](I)[CH2:15][CH3:16].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:13][CH2:12][CH2:11][N:10]([CH:9]=[N:8][C:4]1[NH:3][C:2](=[O:1])[CH:7]=[CH:6][CH:5]=1)[CH2:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 178457528HCID 178457528、化合物

生成物 1

HCID 159470N'-(6-Oxo-1,6-dihydropyridin-2-yl)-N,N-dipropylformimidamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1.8 g (10 mmol) of N-(2-pyridon-6-yl)-N'-propylformamidine and N-(2-hydroxy-6-pyridyl)-N'-propylformamidine, 1.9 g (11 mmol) of propyl iodide and 1.5 g (11.mmol) of potassium carbonate are stirred at 80° for 24 hours in 30 ml of absolute ethanol. The reaction mixture is then filtered and concentrated by evaporation The residue is taken up in methylene chloride, washed with water and then dried over Na2SO4 and concentrated by evaporation. The resulting crude product is purified chromatographically. Crystallisation from methylene chloride/ether yields N-(2-pyridon-6-yl)-N',N'-di-n-propylformamidine and N-(2-hydroxy-6-pyridyl)-N',N'-di-n-propylformamidine having a melting point of 102°-104°.

後処理

  1. filtrationThe reaction mixture is then filtered
  2. concentrationconcentrated by evaporation The residue
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated by evaporation
  6. customThe resulting crude product is purified chromatographically
  7. customCrystallisation from methylene chloride/ether

出典と根拠

ORDレコード
ord-1ac1a6175d71461baf3138effbf546c5
出典データセット
uspto-grants-1989_09
特許番号
US04863938

反応ノート

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