Ammonia → 7-bromo-5-nitroisoquinolin-1(2H)-one
反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][O:8][C:9]2=O)=[C:4]([N+:13]([O-:15])=[O:14])[CH:3]=1.[NH3:16]>CO>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][NH:16][C:9]2=[O:8])=[C:4]([N+:13]([O-:15])=[O:14])[CH:3]=1参加物
4
反応条件
- 温度
- 60 °C
実験手順
A sealed tube containing 7-bromo-5-nitro-1H-isochromen-1-one (293a, 9.20 g, 34.1 mmol) and 7 N ammonia solution in methanol (100 mL) was stirred at 60° C. overnight. After chilling in an ice bath, the resulting precipitate was collected by filtration, washed with cold methanol, and air-dried to give 7-bromo-5-nitroisoquinolin-1(2H)-one (293b, 7.6 g, 83% yield). as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ 11.82 (br. s., 1H), 8.56-8.64 (m, 2H), 7.48 (d, J=7.58 Hz, 1H), 6.89 (d, J=7.58 Hz, 1H). MS: 267/269 [M−1].
後処理
- temperatureAfter chilling in an ice bath
- filtrationthe resulting precipitate was collected by filtration
- washwashed with cold methanol
- customair-dried
出典と根拠
- ORDレコード
- ord-8697ef7c67ca4b70960db1d124b721e8
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040515B2
反応ノート
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