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Methyl iodide → 5-Methoxyadamantan-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Idramantone | HCID 64184 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Methoxyadamantan-2-one | HCID 528352 | — |
反応手順
THF 5 ml solution of 5-hydroxy-2-adamantanone 100 mg and methyl iodide 0.113 ml was cooled at 0° C., and sodium hydride (60%, oil suspension) 48.2 mg was added therein, and the temperature of the reaction mixture was gradually changed to room temperature, then stirred for 25 hours. The reaction mixture was cooled again, and water was added thereto, then THF was removed by concentration in vacuo. The thus obtained residue was extracted with chloroform and dried by adding anhydrous sodium sulfate. After separation of the drying agent, the filtrate was concentrated in vacuo. Residue was purified by means of silica gel column chromatography (Wako gel, C200, n-hexane: ethyl acetate=10:1) to obtain the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05650406 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-1f05df81ea684a0eac2c1f6724f77769 |
| 出典メモ | uspto-grants-1997_07 |