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Acetic Acid → 5,6-Dimethyl-2-(methylsulfanyl)pyrimidin-4(1h)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5,6-Dimethyl-2-thiouracil | HCID 2736249 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5,6-Dimethyl-2-(methylsulfanyl)pyrimidin-4(1h)-one | HCID 135494970 | 64% |
反応手順
To a stirred solution of 5,6-dimethyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (10.0 g, 64.0 mmol, Example 1, Step A) and sodium hydroxide (10.0 g, 260.0 mmol) in water (150 mL) at ambient temperature was added methyl iodide (15.0 g, 320.0 mmol), and the reaction mixture was stirred at ambient temperature overnight. Then the reaction mixture was acidified with acetic acid (50 mL), and the solid was collected by filtration and dried to afford 7.0 g (64%) of the titled compound as a white solid. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.87 (s, 3H), 2.18 (s, 3H), 2.45 (s, 3H), 12.38 (bs, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447051B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-8b9970a145f54e7f8cdb43222681458b |
| 出典メモ | uspto-grants-2016_09 |