Nitric Acid → 4-fluoro-6-nitro-1,3-benzoxazol-2(3H)-one
反応式
[N+:1]([O-:4])(O)=[O:2].[F:5][C:6]1[C:11]2[NH:12][C:13](=[O:15])[O:14][C:10]=2[CH:9]=[CH:8][CH:7]=1>S(=O)(=O)(O)O>[F:5][C:6]1[C:11]2[NH:12][C:13](=[O:15])[O:14][C:10]=2[CH:9]=[C:8]([N+:1]([O-:4])=[O:2])[CH:7]=1参加物
4
反応条件
- 温度
- -10 °C
実験手順
Nitric acid (70%, 2.50 ml, 0.0389 mol) is added dropwise at −10° C. to a solution of 4-fluoro-1,3-benzoxazol-2(3H)-one (Step 4, 5.95 g, 0.0389 mol) in concentrated sulfuric acid (60 ml). The reaction is stirred at −10° C. for 30 minutes and then poured into ice water. The resulting precipitate is collected by filtration and dried under reduced pressure to give desired product contaminated with approximately 10-15% of the undesired 5-nitro isomer (7.2 g, 93%); mp 177-9° C.
後処理
- filtrationThe resulting precipitate is collected by filtration
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-dfec456e8f794131a3ef4e3446e51d3f
- 出典データセット
- uspto-grants-2010_01
- 特許番号
- US07645781B2
反応ノート
読み込み中…