関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | HCID 178507748 | HCID 178507748 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178482205 | HCID 178482205 | — |
反応手順
4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (238 mg, 0.0066 mol), (prepared according to a method analogous to that described in Example 28) is suspended in dichloromethane (5 ml) at 23° C. Triethylamine (0.1 ml, 0.0079 mol) and acetic anhydride (0.062 ml, 0.0066 mol) are added. The mixture is then stirred for 20 hours then evaporated to dryness. The oil obtained is taken up with ethyl acetate and water. After decantation and extraction by ethyl acetate, the organic phase is washed with water then with a saturated solution of sodium chloride, dried over sodium sulphate then the solvent is evaporated off. The residue obtained is adsorbed on silica then purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 7-3 to 9-1). After washing with diisopropyl ether and isopentane, a beige-coloured powder is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07534805B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-84812724710249d4b3aac5f37c78b811 |
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| 出典メモ | uspto-grants-2009_05 |
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