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Diisopropyl Ether → Methyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate sodium salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | 1-(2,6-Dimethoxyphenyl)ethanone | HCID 16267 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Ethanedioic acid, monoethyl ester | HCID 21943339 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate sodium salt | HCID 70245405 | — |
反応手順
A solution of 100 g of 2,6-dimethoxyacetophenone and 7.5 ml of ethyl oxalate in 520 ml of anhydrous MeOH is added slowly to a solution of sodium methylate prepared from 12.7 g of sodium and 285 ml of anhydrous MeOH. The reaction mixture is heated to reflux for 7 hours and left overnight at RT. It is poured into 2 litres of isopropyl ether and left stirring for 15 minutes. The expected product is obtained by filtration, washing with isopropyl ether and drying under vacuum, m=120 g, m.p.=178° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723483 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-33cc46ae4b86423a92b024e4bd6cb9eb |
| 出典メモ | uspto-grants-1998_03 |