関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | HCID 178526243 | HCID 178526243 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Chloro-1H-pyrrolo[2,3-b]pyridine | HCID 11389493 | 135.4% |
反応手順
To a pink solution of 1H-pyrrolo[2,3-b]pyridine 7-oxide (2.47 g, 0.0184 mol) in dimethylformamide (DMF) (13.3 mL, 0.172 mol) was added methanesulfonyl chloride (4.0 mL, 0.052 mol) at 50° C., and the pink color changed to orange. The reaction mixture was heated at 73° C. for 2 h, then cooled to 40° C. Water (35 mL) was added, and the resulting suspension was cooled at 0° C. NaOH was added to adjust the pH of the mixture to about 7. The mixture was filtered and washed with water (×3) to give 3.8 g of a wet pale orange solid that was dried at 40° C. overnight to give the product (2.35 g, 82.2% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541425B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-3e3c3a67cf724308be44647d8de12ac5 |
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| 出典メモ | uspto-grants-2013_09 |
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