4-Amino-3,5-dinitropyridine → Pyridine-3,4,5-triamine
반응식
[N+:1]([C:4]1[CH:5]=[N:6][CH:7]=[C:8]([N+:11]([O-])=O)[C:9]=1[NH2:10])([O-])=O>CCO>[N:6]1[CH:7]=[C:8]([NH2:11])[C:9]([NH2:10])=[C:4]([NH2:1])[CH:5]=1참가 물질
3
실험 절차
3,5-Dinitro-pyridin-4-ylamine 2 (5.00 g, 27 mmol) was suspended in EtOH (80 ml). The flask was evacuated and then purged with a nitrogen atmosphere. To this flask, Pt/C (500 mg of 10%) was added. The flask was re-evacuated, and then placed under a hydrogen atmosphere (40 psi) on a Parr hydrogenator. It was allowed to shake for 18 hours, and was judged complete by TLC. The platinum catalyst was removed by CELITE filtration, and the solvent was removed by evaporation under a reduced atmosphere to yield the title product 3, a brown solid (3.24 g (97%), 27 mmol). 1H NMR (20): δ 7.51 (s, 2H). MS (ESI-POS): [M+H]+=125.
후처리
- customThe flask was evacuated
- custompurged with a nitrogen atmosphere
- additionTo this flask, Pt/C (500 mg of 10%) was added
- customThe flask was re-evacuated
- customThe platinum catalyst was removed by CELITE filtration
- customthe solvent was removed by evaporation under a reduced atmosphere
출처 및 근거
- ORD 기록
- ord-c93441afe0d644aabaf5f7f965d4d73a
- 출처 데이터셋
- uspto-grants-2009_09
- 특허 번호
- US07582634B2
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