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1-(2,6-Dimethoxyphenyl)ethanone → Ethyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate potassium salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(2,6-Dimethoxyphenyl)ethanone | HCID 16267 | — |
| 反応物 | Ethanedioic acid, monoethyl ester | HCID 21943339 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 4-(2,6-dimethoxyphenyl)-4-oxido-2-oxo-3-butenoate potassium salt | HCID 70244972 | — |
反応手順
A solution of 13.4 g of 95% potassium tert-butylate in 72 ml of ethanol is added over 6 minutes to a solution, stirred and heated to 50° C., of 18 g of 2,6-dimethoxyacetophenone in 54 ml of ethanol. The mixture is heated to reflux, 16.3 ml of ethyl oxalate are added over 9 minutes and refluxing is continued for 1 hour. 40 ml of ethanol are then distilled off and the mixture is allowed to cool with stirring for two and a half hours. The mixture is filtered, and the precipitate is washed with 40 ml of ethanol and dried under vacuum at 60° C. for 17 hours to obtain 31 g of expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06172239B2 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-6da63e9d4b604faf86ddf6e0b5b24e35 |
| 出典メモ | uspto-grants-2001_01 |