Phosphorus oxychloride → (1,2-Benzoxazol-3-yl)methanesulfonyl chloride
反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([CH2:10][S:11]([OH:14])(=O)=[O:12])=[N:2]1.P(Cl)(Cl)([Cl:17])=O>>[CH:8]1[CH:9]=[C:4]2[C:3]([CH2:10][S:11]([Cl:17])(=[O:14])=[O:12])=[N:2][O:1][C:5]2=[CH:6][CH:7]=1参加物
3
実験手順
1,2-Benzisoxazole-3-methanesulfonic acid (1) (1.00 g, 4.7 mmol) was mixed with xylenes (10 mL) and phosphorous oxychloride (1.0 mL, 11 mmol) and heated to reflux until the reaction was complete. The mixture was filtered through CELITE™ and evaporated to dryness to yield 1,2-benzisoxazole-3-methanesulfonyl chloride (2) as a light brown solid. It was dissolved in ethyl acetate (10 mL), cooled in an ice-bath and treated with ammonia. Work-up analogous to example 2 gave pure zonisamide.
後処理
- temperatureheated
- temperatureto reflux until the reaction
- filtrationThe mixture was filtered through CELITE™
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-3a5159e2e98f4bbbba596e011308b714
- 出典データセット
- uspto-grants-2008_05
- 特許番号
- US07375233B2
反応ノート
読み込み中…