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Hydrochloric Acid → N*4*-(4-Bromo-phenyl)-6-(5-chloro-2-methoxy-phenyl)-pyrimidine-2,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Bromoaniline | HCID 7807 | — |
| 反応物 | 4-Chloro-6-(5-chloro-2-methoxy-phenyl)-pyrimidin-2-yl-amine | HCID 86004313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N*4*-(4-Bromo-phenyl)-6-(5-chloro-2-methoxy-phenyl)-pyrimidine-2,4-diamine | HCID 11350266 | 98.6% |
反応手順
To a stirred suspension of 4-chloro-6-(5-chloro-2-methoxy-phenyl)-pyrimidin-2-yl-amine (0.054 g, 0.20 mmol) in ethanol (7.5 ml) was added a solution of hydrogen chloride in dioxane (4.0 M, 0.025 ml) followed by 4-bromoaniline (0.069 g, 0.40 mmol). After heating under reflux for 45 minutes, volatiles were removed under reduced pressure. The residue was treated with 1.0 M hydrochloric acid (10 ml) and stirred for 30 minutes. Filtration provided the hydrochloride salt of the title compound (0.08 g, 90% yield). 1H NMR (DMSO-d6) δ 3.90 (s, 3H, CH3), 6.71 (s, 1H, Ar), 7.30 (d, 1H, J=9.0 Hz, Ar), 7.57-7.59 (m, 2H, Ar), 7.65 (dd, 1H, J=9.0 Hz, J=2.4 Hz, Ar), 7.70 (d, 1H, J=2.4 Hz, Ar), 7.80-7.86 (m, 2H, Ar), 11.08 (s, 1H, NH).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07419984B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-03087b78bfff4b379f791079be59971a |
| 出典メモ | uspto-grants-2008_09 |