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Methyl iodide → 6-Iodo-1-(2-methoxyethyl)-2-(methylthio)pyrimidin-4(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-iodo-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one | HCID 86684687 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Iodo-1-(2-methoxyethyl)-2-(methylthio)pyrimidin-4(1H)-one | HCID 86684686 | 43.1% |
反応手順
To a stirring solution of 6-iodo-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (9.00 g, 28.83 mmol) in MeCN (200 mL) was added diisopropylethylamine (5.0 mL, 28.83 mmol) and iodomethane (9.0 mL, 144.17 mmol). The reaction mixture was stirred at room temperature for 18 hours, and concentrated in vacuo. The residue was partitioned ortioned between CH2Cl2 (200 mL) and 1N aqueous HCl (100 mL). The layers were separated and the organic layer was washed with brine (100 mL), dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by hot trituration with CH2Cl2/heptane to give the title compound (4.05 g, 43%) as a cream colored solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841314B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-2ea1b69b5b644f17b66a4f77d405a6f5 |
| 出典メモ | uspto-grants-2014_09 |