反応式
[I:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[I:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]参加物
反応条件
- 温度
- 80 °C
実験手順
2-Iodobenzoic acid (100 g) was dissolved in 400 mL of concentrated sulphuric acid and placed in a 2 liter 3 necked flask. The flask was fitted with reflux condenser, a thermometer and an addition funnel. Fuming nitric acid (400 ml) was added drop by drop. The addition was adjusted in such a way that the temperature was allowed to raise to 80° C. over a period of 2 hours. During the addition, the reaction mixture was stirred vigorously and maintained the temperature at 80° C. for an additional 2 hours. After the completion of the reaction, the reaction mixture was poured slowly into crushed ice (3 Kg). The contents were allowed to settle and were filtered. The yellow precipitate was collected and dried at 30° C. The yield was 9.0 grams.
後処理
- customThe flask was fitted
- temperaturewith reflux condenser
- additionThe addition
- additionDuring the addition
- temperaturemaintained the temperature at 80° C. for an additional 2 hours
- customAfter the completion of the reaction
- additionthe reaction mixture was poured slowly
- filtrationwere filtered
- customThe yellow precipitate was collected
- customdried at 30° C
出典と根拠
- ORDレコード
- ord-2a376a7b17f4460fb434e143b1bcba79
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06780995B2
関連ノート
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