Ammonia → 5-Bromo-4-methylisoquinoline
反応式
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[N:4][CH:3]=1.[Br:12]N1C(=O)CCC1=O.N>S(=O)(=O)(O)O>[Br:12][C:10]1[CH:9]=[CH:8][CH:7]=[C:6]2[C:11]=1[C:2]([CH3:1])=[CH:3][N:4]=[CH:5]2参加物
5
実験手順
4-Methylisoquinoline (0.1 ml, synthesized according to the method described in Tetrahedron. Lett. 34, 45, 7239 (1993)) was dissolved in concentrated sulfuric acid (1 ml), then added with N-bromosuccinimide (125 mg) with ice cooling and stirred for 2 hours. The reaction mixture was added with 28% aqueous ammonia (5 ml) and extracted twice with dichloromethane (10 ml for each time). The organic layer was dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=50:1) to obtain the title compound (108 mg).
後処理
- extractionextracted twice with dichloromethane (10 ml for each time)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (chloroform:methanol=50:1)
出典と根拠
- ORDレコード
- ord-4b5eef1a0b364453826833678fecada6
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07094789B2
反応ノート
読み込み中…