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Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → 3-(Ethoxycarbonylmethyl)-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester | HCID 70670 | — |
| 反応物 | 7-[(4,6-Dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide | HCID 19927417 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(Ethoxycarbonylmethyl)-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide | HCID 19927409 | — |
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 2.5 g of (ethoxycarbonylmethylene)-triphenyl-phosphorane is maintained at reflux temperature for 10 hours in approximately 40 ml of tetrahydrofuran. The solvent is then evaporated off and the reaction material which remains is purified on a column of silica gel (eluant: ethyl acetate/n-hexane 1:1) to yield 3-(ethoxycarbonylmethyl)-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide, m.p. 150°-152° 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-2718d09302a4483d9c03c8a2693c0064 |
| 出典メモ | uspto-grants-1994_07 |