2-Amino-6-chloropyridine-3,5-dicarbonitrile → 2-Aminopyridine-3,5-dicarbonitrile
반응식
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[C:4](Cl)[N:3]=1>[Pd].O1CCOCC1>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[CH:4][N:3]=1참가 물질
4
실험 절차
A mixture of 2-amino-6-chloro-3,5-dicyanopyridine (Synth. Comm. 1993, 2605, 15.0 g, 84 mmol) and 10% palladium on carbon (10.0 g) in dioxane (150 mL) was shaken on a Parr apparatus under hydrogen (55 psi) for 16 h. More catalyst (7.5 g) was added and after a further 4 h the reaction mixture was filtered through celite washing through with ethanol and evaporated in vacuo. The residue was partitioned between methylene chloride and 1 M HCl. The insoluble material was collected by filtration and dried to give the title compound. The methylene chloride layer was washed with brine, dried (Na2SO4) and evaporated in vacuo to give additional product:
후처리
- filtrationwas filtered through celite
- washwashing through with ethanol
- customevaporated in vacuo
- customThe residue was partitioned between methylene chloride and 1 M HCl
- filtrationThe insoluble material was collected by filtration
- customdried
출처 및 근거
- ORD 기록
- ord-a57ce74854b24acfbc7930dae628fd29
- 출처 데이터셋
- uspto-grants-2002_04
- 특허 번호
- US06376499B1
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