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18-Crown-6 → 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-fluoro-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 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 3-Chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide | HCID 19927406 | — |
| 生成物 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-fluoro-phthalide | HCID 19927451 | — |
反応手順
A mixture of 1.0 g of 3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see Example 85) and 0.19 g of spray-dried potassium fluoride and a spatula tip of 18-crown-6 is heated at reflux temperature for 100 minutes. The mixture is then filtered over Celite® and is concentrated by evaporation, and the crude product is recrystallised from ethyl acetate/n-hexane to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-fluoro-phthalide, m.p. 172°-174° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05428002 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-fa7b0110ae764beba36ccd7ed7b688fd |
| 出典メモ | uspto-grants-1995_06 |