関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-(Trifluoromethyl)aniline | HCID 9964 | — |
| 反応物 | 7-Chloro-2-(2,6-dichloro-benzyl)-thiazolo[5,4-d]pyrimidine | HCID 57742463 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | [2-(2,6-Dichloro-benzyl)-thiazolo[5,4-d]pyrimidin-7-yl]-(4-trifluoromethyl-phenyl)-amine | HCID 42642137 | 74% |
反応手順
To a solution of 7-chloro-2-(2,6-dichloro-benzyl)-thiazolo[5,4-d]pyrimidine (45.0 mg, 0.15 mmol) and 4-trifluoromethyl-phenylamine (23 mg, 0.15 mmol) in isopropanol (IPA) (2 mL) was added 1.25 M HCl in IPA (0.26 mL, 0.32 mmol). The resulting solution was heated in a sealed tube to 90° C. After 12 h, the solution was cooled and purified by preparative reverse-phase HPLC to afford the title compound as a colorless solid (50 mg, 74%). MS (ESI): mass calcd. for C19H11Cl2F3N4S, 454.0; m/z found, 455.0 [M+H]+. 1H NMR ((CD3)2SO): 10.46 (s, 1H), 8.58 (s, 1H), 8.19 (d, J=8.5 Hz, 2H), 7.71 (d, J=8.7 Hz, 2H), 7.62 (d, J=8.1 Hz, 2H), 7.47 (dd, J=8.5, 7.8 Hz, 1H), 4.82 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08637527B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-6c8e3ec7d8ba481bbb90572ae8312ea9 |
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| 出典メモ | uspto-grants-2014_01 |
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