Water → 3-Oxo-2,3-dihydro-4H-1,2,4-benzothiadiazine-7-carboxylic acid 1,1-dioxide monohydrate
反応式
[CH3:1][C:2]1[CH:14]=[CH:13][C:5]2[NH:6][C:7](=[O:12])[NH:8][S:9](=[O:11])(=[O:10])[C:4]=2[CH:3]=1.[OH-:15].[Na+].[Mn]([O-])(=O)(=O)=O.[K+].[OH2:23]>>[OH2:10].[O:12]=[C:7]1[NH:6][C:5]2[CH:13]=[CH:14][C:2]([C:1]([OH:23])=[O:15])=[CH:3][C:4]=2[S:9](=[O:11])(=[O:10])[NH:8]1参加物
反応条件
- 温度
- 70 °C
実験手順
7-Methyl-3-oxo-2,3-dihydro-4H-1,2,4-benzothiadiazine 1,1-dioxide (20 g) was suspended in hot water (2000 mL) and supplemented dropwise with a 10% aqueous solution of NaOH until complete dissolution. Potassium permanganate (60 g) was added portionwise and the reaction mixture was stirred for 3 h at 70° C. After cooling, the insoluble material was removed by filtration and the purple filtrate was treated with sodium hydrogen sulfite until complete discolouration of the excess of permanganate. The solution was treated with charcoal, filtered, and the filtrate was adjusted to pH 0 with 12N HCl. The resulting suspension was placed at +4° C. during 2 h and the crystalline precipitate was collected by filtration, washed with water and dried (yield: 14.5 g); m.p.: 305-308° C.
後処理
- temperatureAfter cooling
- customthe insoluble material was removed by filtration
- additionthe purple filtrate was treated with sodium hydrogen sulfite until complete discolouration of the excess of permanganate
- additionThe solution was treated with charcoal
- filtrationfiltered
- waitThe resulting suspension was placed at +4° C. during 2 h
- filtrationthe crystalline precipitate was collected by filtration
- washwashed with water
- customdried (yield: 14.5 g)
出典と根拠
- ORDレコード
- ord-cd044a37076446eb93997208ffdaa446
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06242443B1
反応ノート
読み込み中…