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Dabco → HCID 21081494、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | 4-Chloro-7-methylthieno(3,2-d)pyrimidine | HCID 2777586 | — |
| 反応物 | HCID 21081495 | HCID 21081495 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 21081494 | HCID 21081494 | 31% |
反応手順
To a mixture of 1-(3-fluoro-4-hydroxyphenyl)-3-(2-(4-fluorophenyl)acetyl)thiourea (24 mg, 0.075 mmol, Compound A of Example 3), 4-chloro-7-methylthieno[3,2-d]pyrimidine (13.8 mg, 0.075 mmol, commercially available) and 1,4-diazabicyclo[2.2.2]octane (DABCO, 8.4 mg, 0.075 mmol) was added MeCN (2 mL). The reaction was stirred at RT for 4 h and concentrated in vacuo. The residue was purified by reverse phase preparative HPLC to give the title compound (11.2 mg, 31%) as a white solid. 1H NMR (CDCl3) δ 12.45 (s, 1H), 8.79 (s, 1H), 8.61 (s, 1H), 7.93 (dd, 1H, J=13.8, 2.2 Hz), 7.46 (s, 1H), 7.43 (m, 1H), 7,28 (m, 3H), 7.12 (m, 2H), 3.72 (s, 2H), 2.51 (s, 3H); MS(ESI+) m/z 471 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07173031B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-bc78f8683598467da20f522712729387 |
| 出典メモ | uspto-grants-2007_02 |