Bromine → N-(5-bromo-4-fluoro-2-methoxyphenyl)acetamide
反応式
[Br:1]Br.[F:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:13])[CH3:12])=[C:6]([O:14][CH3:15])[CH:5]=1>C(O)(=O)C>[Br:1][C:9]1[C:4]([F:3])=[CH:5][C:6]([O:14][CH3:15])=[C:7]([NH:10][C:11](=[O:13])[CH3:12])[CH:8]=1参加物
4
実験手順
Bromine (1.8 ml, 34 mmol) was added dropwise to a solution of the product of Step 1 (5.69 g, 31 mmol) in acetic acid (100 ml). After 18 hours at room temperature additional bromine (0.3 ml) was added and the solution stirred for a further 3 hours. The solution was partitioned between water and ethyl acetate and the layers separated. The organic phase was then washed with aqueous sodium thiosulfate solution, water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title compound. MS (ES+) m/e 262/264 [M+H]+.
後処理
- customThe solution was partitioned between water and ethyl acetate
- customthe layers separated
- washThe organic phase was then washed with aqueous sodium thiosulfate solution, water and brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-f574fc3e122143dabe90fc1ef8101837
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07381728B2
反応ノート
読み込み中…