3-Nitrobenzoic acid → 3-Bromo-5-nitrobenzoic acid
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([OH:9])=[O:8])([O-:3])=[O:2].[Br:13]N1C(=O)CCC1=O>S(=O)(=O)(O)O>[Br:13][C:11]1[CH:10]=[C:6]([CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:12]=1)[C:7]([OH:9])=[O:8]参加物
4
反応条件
- 温度
- 60 °C
実験手順
m-Nitrobenzoic acid (11.2 g, 67.0 mmol) was taken up in sulfuric acid (30 mL) and heated to 60° C. To this solution was added N-bromosuccinimide (14.3 g, 80.4 mmol) in three portions each over a 15 minute period. After stirring for 2 h, the mixture was poured into crushed ice (100 g) to precipitate a solid. The solid was filtered, washed with water followed by hexanes to give the desired product (16 g, 97%). LCMS for C7H3BrNO4 (M−H)+: m/z=244.0, 246.0.
後処理
- additionthe mixture was poured
- customto precipitate a solid
- filtrationThe solid was filtered
- washwashed with water
出典と根拠
- ORDレコード
- ord-4bc26b81c9524c55b82a9f4fb88c2f89
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871753B2
反応ノート
読み込み中…