4-Amino-3,5-dinitropyridine → Pyridine-3,4,5-triamine
反応式
[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]=1参加物
3
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-c93441afe0d644aabaf5f7f965d4d73a
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07582634B2
反応ノート
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