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Hydrochloric Acid → 4-(3-Methoxyanilino)-2,6-di(2-pyridinyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Methoxyaniline | HCID 10824 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chloro-2,6-di(2-pyridinyl)pyrimidine | HCID 2767066 | — |
| 溶媒 | Water ethanol | HCID 19096565 | — |
| 生成物 | 4-(3-Methoxyanilino)-2,6-di(2-pyridinyl)pyrimidine | HCID 22732500 | 60.5% |
反応手順
A mixture 4-chloro-2,6-di(2-pyridinyl)pyrimidine (25 mg, 0.093 mmol), m-anisidine (16 μl, 0.140 mmol) and 2N HCl (75 μl) in water:ethanol (2:1, 10 ml) was refluxed for 24 h. The mixture was cooled to room temperature and basified with aqueous 2N NaOH to pH 10-12. The resulting precipitate was filtered, washed with water and aqueous ethanol to give a yellow solid (20 mg, 60%). 1H NMR (CDCl3): 8.87-8.85 (m, 1H), 8.69-8.61 (m, 3H), 7.95 (s, 1H), 7.92-7.84 (m, 2H), 7.44-7.36 (m, 2H), 7.33 (d, J=8.1 Hz, 1H), 7.30 (s, 1H), 7.05 (t, J=2.1 Hz, 1H), 6.98 (dd, J=2.1, 8.1 Hz, 1H), 6.79-6.75 (m, 1H), 3.86 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06716851B2 |
| 出典データセット | uspto-grants-2004_04 |
| ORD ID | ord-1bcb95bd9393417fb4bdfd4d28ea1a12 |
| 出典メモ | uspto-grants-2004_04 |