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18-Crown-6 → 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-thiocyano-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 thiocyanate | HCID 516872 | — |
| 反応物 | 3-Chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide | HCID 19927406 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-thiocyano-phthalide | HCID 19927419 | — |
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 0.46 g of potassium thiocyanate is heated in the presence of a spatula tip of 18-crown-6 in 15 ml of acetonitrile for 4 hours. The mixture is then filtered through Celite®, concentrated by evaporation and chromatographed with 30% ethyl acetate/n-hexane to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-thiocyano-phthalide in the form of light-yellow crystals, m.p. 161°-163° 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-e1efd6f1d85b460595d8335948a61130 |
| 出典メモ | uspto-grants-1995_06 |