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Methyl iodide → 4-Methyl-2-(methylsulfanyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Mercapto-4-methylpyrimidine hydrochloride | HCID 178428687 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Methyl-2-(methylsulfanyl)pyrimidine | HCID 821261 | 86.4% |
反応手順
To a solution of NaOH (7.46 g, 186.4 mmol) in water (120 mL), 4-methylpyrimidine-2-thiol hydrochloride (13.78 g, 84.7 mmol) was added and subsequently iodomethane (13.23 g, 93.2 mmol) was added dropwise under argon atmosphere. It was stirred at room temperature for 2 h. It was extracted with CH2Cl2 (×2). The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford 10.26 g of the desired compound (yield: 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536194B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-28d9962299d84e278f896f2ad27afb03 |
| 出典メモ | uspto-grants-2013_09 |