反応式
Cl.[OH:2][C:3]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][N:4]=1.[Cl:12]([O-])(=O)=O.[K+]>O>[Cl:12][C:8]1[C:3]([OH:2])=[N:4][CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[CH:7]=1参加物
5
反応条件
- 温度
- 53 °C
実験手順
Concentrated hydrochloric acid (239 g) was added to 2-hydroxy-5-nitropyridine (40.0 g). The resulting slurry was heated to 53° C., and stirred until all the solids dissolved. To this was slowly added a solution of potassium chlorate (14.0 g) in water (250 g), while maintaining the temperature between 55° C. and 59° C. The resulting mixture was stirred at 58–62° C. for about 1 hour. The reaction was then cooled to room temperature, stirred for 12 hours and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/DMSO-d6) δ 8.64 (d, J=2.9 Hz, 1H), 8.35 (d, J=2.9 Hz, 1H)
後処理
- dissolutiondissolved
- temperaturewhile maintaining the temperature between 55° C. and 59° C
- stirringThe resulting mixture was stirred at 58–62° C. for about 1 hour
- temperatureThe reaction was then cooled to room temperature
- stirringstirred for 12 hours
- filtrationfiltered
- washAfter washing the wet cake with water
- customthe product was dried in a vacuum oven
出典と根拠
- ORDレコード
- ord-e742666630e141e199317d1c97597e3b
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07354937B2
関連ノート
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