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m-Chloroperbenzoic acid → 1-(10,10-Dioxophenoxathiin-2-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 2-Acetylphenoxathiin | HCID 515174 | — |
| 反応物 | Calcium Hydroxide | HCID 6093208 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(10,10-Dioxophenoxathiin-2-yl)ethanone | HCID 515177 | 75.6% |
反応手順
To a solution of 2-acetyl phenoxathiin (J.A.C.S. 1936, 58, 717) (484 mg, 2 mmol) in methylene chloride (25 mL) there was added 85% m-chloroperoxy benzoic acid (MCPBA 1.015 g, 5 mmol) and the mixture stirred at room temperature. After 3 hours, more MCPBA was added (250 mg) and stirring was continued for a further hour. Enough methylene chloride was added to dissolve the solids, followed by calcium hydroxide (3 g); after stirring for a further 5 minutes, the mixture was filtered and the filtrate evaporated to a solid residue which was triturated with ether (10 mL) and filtered to afford the sulfone (415 mg) as a white solid, m.p.: 163°-165° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05036067 |
| 出典データセット | uspto-grants-1991_07 |
| ORD ID | ord-16f1a8e4dc1243019f1f737c05877b79 |
| 出典メモ | uspto-grants-1991_07 |