N-methyl-2-pyrrolidone → 3-Aminopyridine-2-carbonitrile
반응식
[NH2:1][C:2]1[C:3](Cl)=[N:4][CH:5]=[CH:6][CH:7]=1.[CH3:9][N:10]1CCCC1=O>>[NH2:1][C:2]1[C:3]([C:9]#[N:10])=[N:4][CH:5]=[CH:6][CH:7]=1참가 물질
3
반응 조건
- 온도
- 185 °C
실험 절차
A mixture of 3-Amino-2-chloro-pyridine (5 g) and cuprous cyanide (5 g) in 10 mL of N-Methylpyrrolidone was heated with stirring at 185° C. for 2 h under an atmosphere of nitrogen. The reaction mixture was concentrated in vacuo and concentrated ammonium hydroxide and 10% methanol/methylene chloride were added. The mixture was shaken and filtered, the organic layer separated and the aqueous layer extracted two times with methanol/methylene chloride. The combined organic extracts were dried over magnesium sulfate and the solvent removed in vacuo. The residue was recrystallized from ethyl acetate/hexane to afford 3-Amino-2-cyanopyridine as a tan solid
후처리
- temperaturewas heated
- concentrationThe reaction mixture was concentrated in vacuo and concentrated ammonium hydroxide and 10% methanol/methylene chloride
- additionwere added
- stirringThe mixture was shaken
- filtrationfiltered
- customthe organic layer separated
- extractionthe aqueous layer extracted two times with methanol/methylene chloride
- dry with materialThe combined organic extracts were dried over magnesium sulfate
- customthe solvent removed in vacuo
- customThe residue was recrystallized from ethyl acetate/hexane
출처 및 근거
- ORD 기록
- ord-fbffb0a1d8894513b8ee9de8211916be
- 출처 데이터셋
- uspto-grants-1993_05
- 특허 번호
- US05212310
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