Ammonia → 2-Chloro-6-methoxyquinolin-4-amine
反応式
[Cl:1][C:2]1[CH:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1.CO.[NH3:17]>>[Cl:1][C:2]1[CH:11]=[C:10]([NH2:17])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1参加物
4
反応条件
- 温度
- 150 °C
実験手順
A suspension of 2,4-dichloro-6-methoxyquinoline (5.00 g, 22.0 mmol) in NH3 (g)/MeOH (saturated, 40 mL) was heated to 150° C. for 16 hours in a sealed tube. The solvent was removed and the residue was diluted with MeOH (20 mL). The mixture was filtered off and the filtrate was concentrated to give the crude product. Purification by column chromatography on silica gel (PE/EtOAc=2/1) gave product (7.50 g, yield: 55%) as a solid.
後処理
- customThe solvent was removed
- additionthe residue was diluted with MeOH (20 mL)
- filtrationThe mixture was filtered off
- concentrationthe filtrate was concentrated
- customto give the crude product
- customPurification by column chromatography on silica gel (PE/EtOAc=2/1)
出典と根拠
- ORDレコード
- ord-3d078d335c5d4208b8e5a167dfcb8f7b
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08921562B2
反応ノート
読み込み中…