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Hydrochloric Acid → (R)-3-(3,5-dimethylbenzoyl)-4-methyldihydrofuran-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzoic acid, 3,5-dimethyl-, methyl ester | HCID 32786 | — |
| 反応物 | (R)-4-Methyldihydrofuran-2(3H)-one | HCID 5325910 | — |
| 生成物 | (R)-3-(3,5-dimethylbenzoyl)-4-methyldihydrofuran-2-one | HCID 53860757 | 62.1% |
反応手順
To a solution of (R)-4-methyldihydrofuran-2-one (1.68 g in 40 mL dioxane) were added 5.51 g 3,5-dimethylbenzoic acid methyl ester followed by 1.82 g sodium hydroxide and the mixture heated to reflux on an oil bath. After 3 hours, the mixture was cooled to room temperature and the pH neutralized by the addition of 0.5N hydrochloric acid. The mixture was then extracted with ethyl acetate and the organic portion washed with brine and dried over sodium sulfate. Purification of the concentrate by flash chromatography on silica gel (hexane:ethyl acetate, 9:1) gave the title compound (2.42 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06159975 |
| 出典データセット | uspto-grants-2000_12 |
| ORD ID | ord-592d5046b75a4bc3bbd6e7b836cf57c2 |
| 出典メモ | uspto-grants-2000_12 |