関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1H-Pyrrolo(2,3-b)pyridine | HCID 9222 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178526243 | HCID 178526243 | — |
反応手順
539.7 g (2.35 mol) of 3-chloroperbenzoic acid are dissolved in 6.11 l of dichloromethane, and water that separates off is removed. The organic phase is dried over sodium sulfate and cooled to 0° C. A solution of 163 g (1.38 mol) of 1H-pyrrolo[2,3-b]pyridine in 1.00 l of dichloromethane is then added, and the temperature is allowed to increase to room temperature. After 2 hours, sufficient methanol to re-dissolve the precipitate formed is added. The mixture is filtered through silica gel (mobile phase: dichloromethane/methanol 95:5) and the product fractions are dried after concentration under high vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737153B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-9895e424d20e49a3b999223b13d4f924 |
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| 出典メモ | uspto-grants-2010_06 |
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