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Hydrochloric Acid → 6-Chloro-4-(1H-pyrrolo[2,3-b]pyridin-3-yl)-2-pyridinamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N-(6-chloro-4-(1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)pyridin-2-yl)acetamide | HCID 87192560 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Chloro-4-(1H-pyrrolo[2,3-b]pyridin-3-yl)-2-pyridinamine | HCID 49830311 | 67.7% |
反応手順
A mixture of Example 91a (186.0 mg, 0.436 mmol) and HCl (0.20 mL, 6.6 mmol) in ethanol (6 mL) was heated at 95° C. for 3 hours and cooled. Half of the solvent was evaporated; the resulting suspension was filtered and washed with EtOH. The solids were stirred in saturated NaHCO3 for 30 minutes, filtered, washed with water, and oven-dried to give 72.2 mg of the title compound. 1H NMR (300 MHz, DMSO-d6) ppm 6.30 (s, 2H), 6.85 (s, 1H), 6.91 (s, 1H), 7.15 (m, 1H), 8.12 (s, 1H), 8.21-8.36 (m, 2H), 12.15 (s, brd, 1H). MS (ESI+) m/z 244.8 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08435980B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-9c1a469b91da4e979b760434c42ef1fc |
| 出典メモ | uspto-grants-2013_05 |