Ammonia → 7-Fluoro-1,3-benzothiazol-2-amine
反応式
[F:1][C:2]1[C:10]2[S:9][C:8](S(C)(=O)=O)=[N:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[NH3:15]>C(O)C>[NH2:15][C:8]1[S:9][C:10]2[C:2]([F:1])=[CH:3][CH:4]=[CH:5][C:6]=2[N:7]=1参加物
4
反応条件
- 温度
- 160 °C
実験手順
A mixture of 7-fluoro-2-methylsulfonyl-1,3-benzothiazole (500 mg, 2.16 mmol) in 10 mL ethanol and 20% ethanolic ammonia (20 mL) was heated at 160° C. in a sealed tube for 12 h. It was cooled to RT, ethanol was removed under reduced pressure, and the brownish residue was purified by column chromatography (5% to 10% methanol in methylene chloride) to afford the title compound. 1H-NMR (CDCl3, 300 MHz): δ=7.35 (d, J=7.5 Hz, 1H), 7.33-7.37 (m, 1H), 6.93-6.84 (m, 1H), 5.30 (brs, 2H).
後処理
- temperatureIt was cooled to RT
- customethanol was removed under reduced pressure
- customthe brownish residue was purified by column chromatography (5% to 10% methanol in methylene chloride)
出典と根拠
- ORDレコード
- ord-fbd7008f0aec4d6c826646992077952a
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08178668B2
反応ノート
読み込み中…