Potassium Carbonate → N'-(6-Oxo-1,6-dihydropyridin-2-yl)-N,N-dipropylformimidamide
반응식
[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]참가 물질
5
실험 절차
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°.
후처리
- filtrationThe reaction mixture is then filtered
- concentrationconcentrated by evaporation The residue
- washwashed with water
- dry with materialdried over Na2SO4
- concentrationconcentrated by evaporation
- customThe resulting crude product is purified chromatographically
- customCrystallisation from methylene chloride/ether
출처 및 근거
- ORD 기록
- ord-1ac1a6175d71461baf3138effbf546c5
- 출처 데이터셋
- uspto-grants-1989_09
- 특허 번호
- US04863938
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