Sodium Hydroxide → 6-Iodo-4-methylpyridin-3-amine
反応式
Cl[Sn]Cl.O.[I:5][C:6]1[CH:11]=[C:10]([CH3:12])[C:9]([N+:13]([O-])=O)=[CH:8][N:7]=1.[OH-].[Na+]>CCOC(C)=O>[I:5][C:6]1[CH:11]=[C:10]([CH3:12])[C:9]([NH2:13])=[CH:8][N:7]=1参加物
5
実験手順
To a solution of SnCl2.H2O (20.5 g, 108 mmol) in EtOAc (200 mL) was added 2-iodo-4-methyl-5-nitropyridine (5.7 g, 21.6 mmol) in EtOAc (20 mL). Heat was released, and the reaction mixture was kept at reflux for 2 hr. After cooling to rt, the reaction mixture was treated with 50% NaOH (50 mL). Solid was filtered off and washed with EtOAc. The filtrate was washed with brine, dried, and concentrated to afford 2-iodo-4-methyl-5-pyridinamine (5 g, 99%) as a yellow solid.
後処理
- temperatureHeat
- temperatureat reflux for 2 hr
- filtrationSolid was filtered off
- washwashed with EtOAc
- washThe filtrate was washed with brine
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-bbbbf47f9c13471fbab8bdaeb0ef81e0
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08198456B2
反応ノート
読み込み中…