関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Methylbenzeneethanamine | HCID 11503 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | HCID 58872694 | HCID 58872694 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-(N-methylphenethylamino)-6-phenylpyrimidine-4-carboxamide | HCID 15603546 | 51.7% |
反応手順
2-Methanesulfonyl-6-phenylpyrimidine-4-carboxamide (70 mg, 0.25 mmol), 1,4-dioxane (4 mL), DIPEA (0.3 mL, 2.0 mmol) and N-methylphenethylamine (82 mg, 0.6 mmol) were added to a 8 mL vial. The vial was sealed and heated at 85° C. for two days. The reaction mixture was allowed to cool to room temperature, and the solvent then removed by centrifugal evaporation. The residue was purified by preparative HPLC to afford 43 mg of 2-(N-methylphenethylamino)-6-phenylpyrimidine-4-carboxamide. 1H NMR (CDCl3, 300 MHz) δ 8.14 (m, 2H), 7.74 (s, 1H), 7.67 (br s, 1H), 7.47 (m, 3H), 7.25 (m, 5H), 5.79 (br s, 1H), 3.95 (t, J=6.9 Hz, 2H), 3.21 (s, 3H), 2.97 (t, J=6.9 Hz, 2H). HPLC ret. time 3.25 min, 10-100% CH3CN, 5 min run. ESI-MS m/z 333.3 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822451B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-0539cb802972482dbf0f1709587fadb3 |
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| 出典メモ | uspto-grants-2014_09 |
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