反応式
[S:1]1[CH:5]=[CH:4][C:3]2[C:6](=[O:10])[CH2:7][CH2:8][CH2:9][C:2]1=2.[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[N+:11]([C:5]1[S:1][C:2]2[CH2:9][CH2:8][CH2:7][C:6](=[O:10])[C:3]=2[CH:4]=1)([O-:13])=[O:12]参加物
4
反応条件
- 温度
- 0 °C
実験手順
6,7-Dihydrobenzo[b]thiophen-4(5H)-one (5 g, 32.9 mmol) was dissolved in concentrated sulphuric acid (30 mL) and cooled to 0° C. in an ice/salt bath. Concentrated nitric acid (3.5 mL) in concentrated sulphuric acid (20 mL) was added drop-wise keeping the temperature of the reaction below 0° C. The reaction mixture was stirred at 0-5° C. for 1 hr. The solution was poured onto ice and the resulting solid filtered, washed with water and dried in a vacuum oven, affording the title compound (5.68 g, 88%).
後処理
- customthe temperature of the reaction below 0° C
- additionThe solution was poured onto ice
- filtrationthe resulting solid filtered
- washwashed with water
- customdried in a vacuum oven
出典と根拠
- ORDレコード
- ord-6fc7873fef5b46f185c90ef1d6a6da18
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09233982B2
関連ノート
読み込み中…