関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Potassium Permanganate | HCID 516875 | — |
| 反応物 | N-(4,5,6,7-Tetrahydrobenzo[b]thiophen-4-yl)acetamide | HCID 4976773 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Acetamide, N-(4,5,6,7-tetrahydro-7-oxobenzo[b]thien-4-yl)- | HCID 106675 | 73.6% |
反応手順
Acetone (200 ml), N-(4,5,6,7-tetrahydrobenzo[b]-thien-4-yl) acetamide (9.75 g, 0.05 mol) and magnesium sulfate (21.0 g, 0.17 mol) are mixed, stirred and cooled to 10° C. Next, 150 ml of an aqueous potassium permanganate solution (prepared from 21.0 g, 0.133 mol of potassium permanganate and 200 ml of water) is added over 15 minutes to the above mixture, and the whole stirred for 3 hours. After 3 hours reaction time, analysis of the mixture by high pressure liquid chromatography (HPLC) indicates the reaction to be incomplete. The remainder of the above potassium permanganate solution (~50 ml) is added and the reaction mixture stirred for two more hours. Isopropanol (20 ml) is then added, the reaction mixture stirred overnight, and filtered. HPLC analysis of the filtered solution indicates a 73.6% yield of title product, and also the presence of 2% of starting material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04254268 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-2393d935f34849278ec1060f71ea4d4e |
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| 出典メモ | uspto-grants-1981_03 |
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