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Hydrochloric Acid → [2-(2-Chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Nitrophenethylamine | HCID 95153 | — |
| 反応物 | 3-{6-[2-(2,4-Dichloro-phenyl)-ethylamino]-2-methoxy-pyrimidin-4-yl}-phenol | HCID 11494834 | — |
| 反応物 | [2-(2-Chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine | HCID 57636022 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | [2-(2-Chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine hydrochloride | HCID 69073584 | 60% |
反応手順
By proceeding in a similar manner to Example 43(b) but (i) substituting 2-(2-chloro-6-fluoro-phenyl)-ethylamine for 2-(4-nitro-phenyl)-ethylamine, acetonitrile for EtOH as solvent in Step 3 there is prepared [2-(2-chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine which is dissolved in ether and treated with 1 M hydrogen chloride in ether to afford [2-(2-chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine hydrochloride [51 mg, 60%, Example 43(d)] as a solid. LC/MS: RT=2.82 minutes MS: 388 (M+H). 1H NMR [300 MHz, (CD3)2SO]: □7.12-7.48 (7H, m), 6.6 (1H, s), 3.99 (3H, s), 3.82 (3H, s), 3.67 (2H, m), 3.07 (2H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08193183B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-d6b9edde907644119e3a00e6b2e073cb |
| 出典メモ | uspto-grants-2012_06 |