Water → 4-Bromo-7-fluoro-1,2-dihydroisoquinolin-1-one
反応式
[Br:1]Br.[F:3][C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[CH:9][N:10](C)[C:11]2=[O:14])=[CH:6][CH:5]=1.O>C(O)(=O)C>[Br:1][C:8]1[C:7]2[C:12](=[CH:13][C:4]([F:3])=[CH:5][CH:6]=2)[C:11](=[O:14])[NH:10][CH:9]=1参加物
5
反応条件
- 温度
- 26 °C
実験手順
Bromine (3.8 g, 24 mmol) in acetic acid (6 mL) was added slowly to a mixture of 7-fluoro-2-methylisoquinolin-1-one (4 g, 22.4 mmol) in acetic acid (8 mL) at 0° C. After stirring at 26° C. for 2 h, the mixture was poured into water (100 mL) and the solid was collected by filtration. Purification by silica gel chromatography (PE:EA=20:1) gave the title compound (1.4 g, 44%) as an off-white solid. 1H NMR (CDCl3, 400 MHz) δ 8.11 (d, J=9.2 Hz, 1H), 7.84 (dd, J1=9.6 Hz, J2=4.8 Hz, 1H), 7.49-7.45 (m, 1H), 7.34 (s, 1H), 3.62 (3H, s). LCMS: 255.9 [M+H]+
後処理
- filtrationthe solid was collected by filtration
- customPurification by silica gel chromatography (PE:EA=20:1)
出典と根拠
- ORDレコード
- ord-4817ac614cdc40c08c21ac25a573d068
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034900B2
反応ノート
読み込み中…