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18-Crown-6 → 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-phenoxy-phthalide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 3-Chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide | HCID 19927406 | — |
| 反応物 | Potassium phenoxide | HCID 23670670 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-phenoxy-phthalide | HCID 19927487 | — |
反応手順
A mixture of 1.4 g of 3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see Example 85) and 0.63 g of potassium phenolate is heated at reflux temperature in the presence of a spatula tip of 18-crown-6 in 15 ml of acetonitrile. After 19 hours, the reaction mixture is filtered through Celite® and concentrated by evaporation, and the crude product is purified by column chromatography (eluant 25% ethyl acetate/n-hexane) to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-phenoxy-phthalide in the form of white crystals, m.p. 155°-157° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05332717 |
| 出典データセット | uspto-grants-1994_07 |
| ORD ID | ord-0271a6d3e111443db6b1d992f1aeae74 |
| 出典メモ | uspto-grants-1994_07 |