Methyl 6-methoxy-5-nitronicotinate → Methyl 5-amino-6-methoxypyridine-3-carboxylate
反応式
[CH3:1][O:2][C:3]1[C:12]([N+:13]([O-])=O)=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][N:4]=1.[H][H]>C(OCC)(=O)C.[Pd]>[NH2:13][C:12]1[C:3]([O:2][CH3:1])=[N:4][CH:5]=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8]参加物
5
実験手順
A solution of methyl 6-methoxy-5-nitronicotinate (5.4 g) in ethyl acetate (120 mL) is hydrogenated using 5% palladium on carbon (1 g) as catalyst. When hydrogen uptake ceased the mixture is filtered through a pad of diatomaceous earth and the filtrate evaporated. The residue is triturated with n-pentane and methyl t-butyl ether to give methyl 5-amino-6-methoxynicotinoate (4.3 g) as a light-brown solid, m.p.108-9° C. [Elemental analysis: C, 52.99; H, 5.49; N, 15.25%. calculated: C, 52.74; H, 5.53; N, 15.38%.]
後処理
- filtrationis filtered through a pad of diatomaceous earth
- customthe filtrate evaporated
- customThe residue is triturated with n-pentane and methyl t-butyl ether
出典と根拠
- ORDレコード
- ord-eec50a2b617b42dbb6c375beff770400
- 出典データセット
- uspto-grants-2002_10
- 特許番号
- US06472412B1
反応ノート
読み込み中…