関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thioxanthene | HCID 67495 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Thioxanthene, 10,10-dioxide | HCID 596953 | — |
反応手順
Thioxanthene, 29 (2.9 g, 14.6 mmol) was dissolved in glacial acetic acid (90 mL). While under argon, the solution was treated with hydrogen peroxide (6.12 mL, 62.9 mmol of a 35% by wt water solution) and the reaction stirred at 100° C. for 1.5 hr. The reaction was cooled to room temperature, poured into water (250 mL), stirred 0.5 hrs and filtered to give a white solid. The solid was dissolved in CH2Cl2, washed with 5% sodium bisulfite (aq), dried over Na2SO4, filtered and concentrated to dryness in vacuo. Treatment of the resulting oil with methanol gave the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06387893B1 |
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| 出典データセット | uspto-grants-2002_05 |
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| ORD ID | ord-9cc4e73a11a64dd0b7bc01f03e0e4bd8 |
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| 出典メモ | uspto-grants-2002_05 |
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