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Methyl iodide → 7-[3-(2-Methoxyphenyl)pyrazol-1-yl]heptanoic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 7-[3-(2-Hydroxyphenyl)pyrazol-1-yl]heptanoic acid ethyl ester | HCID 136206529 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 7-[3-(2-Methoxyphenyl)pyrazol-1-yl]heptanoic acid ethyl ester | HCID 68488990 | 76% |
反応手順
Add sodium hydride (900 mg, 18 mmol, 60% suspension in mineral oil) to a suspension of 7-[3-(2-hydroxyphenyl)pyrazol-1-yl]heptanoic acid ethyl ester (4.73 g, 15 mmol) and iodomethane (1.1 mL, 18 mmol) in THF (70 mL) at 0° C. under nitrogen and warm the mixture to room temperature to stir for 12 hours. Remove the solvent under reduced pressure, dilute the residue with ethyl acetate (150 mL), wash with water (100 mL), and dry over sodium sulfate. Remove the solvent under reduced pressure and purify the residue by flash column chromatography on silica gel, eluting with hexanes/ethyl acetate (9:1), to provide 7-[3-(2-Methoxyphenyl)pyrazol-1-yl]heptanoic acid ethyl ester (3.75 g, 76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08765796B2 |
| 出典データセット | uspto-grants-2014_07 |
| ORD ID | ord-04771c1af57a4789b53e063626bfb235 |
| 出典メモ | uspto-grants-2014_07 |