4-Methylamino-3-nitroquinoline → 3-Amino-4-(methylamino)quinoline
反応式
[CH3:1][NH:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]=[CH:5][C:4]=1[N+:13]([O-])=O>C(O)C.[Pd]>[NH2:13][C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:3]=1[NH:2][CH3:1])=[CH:11][CH:10]=[CH:9][CH:8]=2参加物
4
実験手順
A suspension of 1.7 g of 4-methylamino-3-nitroquinoline in 75 ml of ethanol is hydrogenated in the presence of 300 mg of 10% palladium on carbon at atmospheric pressure. After hydrogen absorption is complete, the catalyst is removed by filtration and the filtrate is concentrated in vacuo. The residue is purified by column chromatography on silica gel. Elution with chloroform-methanol (2:1 v/v) affords 600 mg (41%) of 3-amino-4-methylaminoquinoline A15 as an oil.
後処理
- customAfter hydrogen absorption
- customthe catalyst is removed by filtration
- concentrationthe filtrate is concentrated in vacuo
- customThe residue is purified by column chromatography on silica gel
- washElution with chloroform-methanol (2:1 v/v)
出典と根拠
- ORDレコード
- ord-025ef8fb61934d759fc6cef98b1fbb90
- 出典データセット
- uspto-grants-1988_06
- 特許番号
- US04753951
反応ノート
読み込み中…