Hydrogen Bromide → 6-Chloro-3,3-dimethyl-benzo[1,4]oxathiin-2-one
反応式
CO[C:3](=[O:17])[C:4]([S:7][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[O:15]C)([CH3:6])[CH3:5].Br>>[Cl:14][C:12]1[CH:11]=[CH:10][C:9]2[O:15][C:3](=[O:17])[C:4]([CH3:5])([CH3:6])[S:7][C:8]=2[CH:13]=1参加物
3
実験手順
To 2-(5-chloro-2-methoxy-phenylsulfanyl)-2-methyl-propionic acid methyl ester (prepared from 5-chloro-2-methoxy-benzenesulfonyl chloride: Syn. Comm., (2001), 31, 505–510) (0.25 g, 0.9 mmol) was added 48% hydrobromic acid (5 ml). The reaction was heated to reflux for 24 hours at which time the solvent was removed by evaporation. To the crude acid phenol was added toluene (5 ml) and catalytic pyridinium p-toluenesulfonate. After 12 hours of heating at reflux the reaction was concentrated and the title compound was isolated by chromatography on silica gel (0.27 g).
後処理
- temperatureThe reaction was heated
- temperatureto reflux for 24 hours at which time the solvent
- customwas removed by evaporation
- additionTo the crude acid phenol was added toluene (5 ml) and catalytic pyridinium p-toluenesulfonate
- temperatureAfter 12 hours of heating
- temperatureat reflux the reaction
- concentrationwas concentrated
出典と根拠
- ORDレコード
- ord-7dff17e2356f4c31aafbe369d51ba4d7
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07098212B2
反応ノート
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