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5-Iodo-6-methylpyrimidine-2,4-diamine → 3-(2,4-Diamino-6-methylpyrimidin-5-yl)-1-(3,4,5-trimethoxyphenyl)prop-2-yn-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Iodo-6-methylpyrimidine-2,4-diamine | HCID 15855792 | — |
| 反応物 | 1-(3,4,5-Trimethoxyphenyl)-2-propyn-1-ol | HCID 16110327 | — |
| 生成物 | 3-(2,4-Diamino-6-methylpyrimidin-5-yl)-1-(3,4,5-trimethoxyphenyl)prop-2-yn-1-ol | HCID 16110328 | 80% |
反応手順
2,4-Diamino-5-iodo-6-methylpyrimidine (250 mg) was allowed to react with 1-(3,4,5-Trimethoxyphenyl)prop-2-yn-1-ol (444 mg) as per the general procedure to afford 3-(2,4-Diamino-6-methylpyrimidin-5-yl)-1-(3,4,5-trimethoxyphenyl) prop-2-yn-1-ol as a yellow powder (275 mg, 80%): Rf=0.12 (9:1, CHCl3:MeOH); mp=174-176° C.; 1H NMR (DMSO-d6) δ 6.85 (s, 2H), 6.27 (s, 2H), 5.98 (d, J) 5.6 Hz, 1H), 5.53 (d, J) 5.4 Hz, 1H), 3.78 (s, 6H), 3.65 (s, 3H), 2.19 (s, 3H), 1.51 (d, J) 7.1 Hz, 3H); 13C NMR (DMSO-d6) δ 167.1, 164.3, 161.2, 152.7, 138.3, 136.7, 103.7, 99.1, 87.9, 79.5, 63.6, 60.0, 55.8, 22.5; HRFAB [M+Li] 351.1638 (calculated C17H20N4O4Li: 351.1645).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08853228B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-a5a86a06e1bc4ff8b8b891ee57eea29b |
| 出典メモ | uspto-grants-2014_10 |