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2-Amino-4-methylpyridine → 2-(5-methyl-2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)-N-(4-methyl-pyridin-2-yl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-4-methylpyridine | HCID 1533 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(5-Methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-yl)acetic acid | HCID 853753 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(5-methyl-2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)-N-(4-methyl-pyridin-2-yl)acetamide | HCID 24745170 | — |
反応手順
A mixture of 2-(5-methyl-2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)acetic acid (75 mg, 0.4 mmol), 4-methylpyridin-2-amine (44 mg, 0.4 mmol), HBTU (151 mg, 0.4 mmol) and 0.1 mL of Et3N in DMF (5 mL) was stirred at room temperature for 2 hours to provide the title compound, which was then purified by HPLC. 1H NMR (400 MHz, DMSO-d6) δ: 11.37 (s, 1H), 10.97 (s, 1H), 8.20 (d, J=8.0 Hz, 1H), 7.81 (s, 1H), 7.51 (s, 1H), 7.03 (d, J=8.0 Hz, 1H), 4.58 (s, 2H), 2.33 (s, 3H), 1.77 (s, 3H). [M+H] calc'd for C13H14N4O2, 275; found, 275.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08034822B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-45ccae9971ee40cc8e3ac3e0296fb6a9 |
| 出典メモ | uspto-grants-2011_10 |