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Sodium Iodide → 3-Cyanomethoxy-7-[(4,6-dimethoxypyrimidin-2-yl)oxy]-phthalide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Chloroacetonitrile | HCID 7856 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide | HCID 19927417 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 3-Cyanomethoxy-7-[(4,6-dimethoxypyrimidin-2-yl)oxy]-phthalide | HCID 19927425 | — |
反応手順
A mixture of 1.5 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) and 0.8 ml of chloroacetonitrile is maintained at 60° C. for 1 hour in ethyl methyl ketone in the presence of 2.1 g of dry potassium carbonate and a spatula tip each of sodium iodide and 18-crown-6. When the reaction material has cooled, it is taken up in tert-butyl methyl ether and the solution is washed with dilute hydrochloric acid and water, concentrated by evaporation and purified by chromatography on silica gel (eluant: ethyl acetate/n-hexane 1:1) to yield 3-cyanomethoxy-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide, m.p. 99°-102° 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-e37d68f706bd42cbb3420ee6f343d04d |
| 出典メモ | uspto-grants-1995_06 |