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Methyl iodide → 1-(4-Acetylamino-5-chloro-2-methoxyphenyl)-5-chloropentan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(4-Acetylamino-5-chloro-2-hydroxyphenyl)-5-chloropentan-1-one | HCID 19081879 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 1-(4-Acetylamino-5-chloro-2-methoxyphenyl)-5-chloropentan-1-one | HCID 19081861 | 67.7% |
反応手順
1-(4-Acetylamino-5-chloro-2-hydroxyphenyl)-5-chloropentan-1-one (1.07 g, 3.5 mmol), potassium carbonate (1.38 g, 10.0 mmol) and iodomethane (0.62 mL, 10.0 mmol) were combined in methyl ethyl ketone (20 mL) and stirred at reflux temperature for 4 hours, 15 minutes. The mixture was partitioned between ethyl acetate and water. The ethyl acetate layer was separated, washed in brine, dried over sodium sulfate, and then evaporated to leave a solid residue. Crystallization of the residue from ethyl acetate-hexanes gave 1-(4-acetylamino-5-chloro-2-methoxyphenyl)-5-chloro-pentan-1-one (0.720 g, 2.37 mmol), m.p. 98°-100° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05763458 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-12c40d93e8884fb3b03071ddda14a120 |
| 出典メモ | uspto-grants-1998_06 |