Methanesulfonyl chloride → HCID 178477812、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[N:11]=[CH:10][NH:9][C:5]2=[N+:6]([O-])[CH:7]=1.CS([Cl:16])(=O)=O.C(=O)([O-])O.[Na+]>CN(C)C=O>[Br:1][C:2]1[C:3]([Cl:16])=[C:4]2[N:11]=[CH:10][NH:9][C:5]2=[N:6][CH:7]=1参加物
5
反応条件
- 温度
- 73 °C
実験手順
6-Bromo-3H-imidazo[4,5-b]pyridine 4-oxide (1.88 g, 8.82 mmol) in N,N-dimethylformamide (12 mL) was heated to 50° C., mixed with methansulfonyl chloride (8.00 mL, 103 mmol) and stirred at 73° C. for 3 hours. The reaction mixture was cooled with ice and gradually poured into saturated aqueous sodium hydrogen carbonate (75 mL), and the precipitated solid was collected by filtration, washed with water and chloroform and dried under reduced pressure to give the title compound as a dark brown solid (1.07 g, yield 52%).
後処理
- temperatureThe reaction mixture was cooled with ice
- filtrationthe precipitated solid was collected by filtration
- washwashed with water and chloroform
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-99b09c1769904fb2808fc4a13284a878
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216999B2
反応ノート
読み込み中…