p-Toluenesulfonic acid monohydrate → HCID 18759913、化合物
反応式
[S:1]1(=[O:13])(=[O:12])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4](=[O:11])[CH2:3][NH:2]1.O.[C:15]1(C)C=CC(S(O)(=O)=O)=CC=1.C([O-])([O-])OC>CO>[CH3:15][O:11][C:4]1[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[S:1](=[O:12])(=[O:13])[NH:2][CH:3]=1参加物
5
実験手順
A mixture of 1.97 g (10 mmol) of 3,4-dihydro-2H-1,2-benzothiazin-4-one 1,1-dioxide, 500 mg (2.6 mmol) of p-toluenesulfonic acid monohydrate, 20 ml of methyl orthoformate and 20 ml of methanol was refluxed for 3 hours. The solvent was distilled off and the residue was purified by chromatography on a silica gel column (eluent: methylene chloride:ethyl acetate=40:1), whereby 2.06 g of the title compound were obtained (yield: 97%).
後処理
- temperaturewas refluxed for 3 hours
- distillationThe solvent was distilled off
- customthe residue was purified by chromatography on a silica gel column (eluent: methylene chloride:ethyl acetate=40:1)
出典と根拠
- ORDレコード
- ord-83247671dadb44c0a688b78a6be53a4c
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06316442B1
反応ノート
読み込み中…