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Sodium Sulfate → 3,5-Dimethyl-4-(hydroxymethyl)isoxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Ethyl 3,5-dimethylisoxazole-4-carboxylate | HCID 736348 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3,5-Dimethyl-4-(hydroxymethyl)isoxazole | HCID 289575 | 75.7% |
反応手順
To a suspension of 23.53 g of lithium aluminum hydride in 600 ml of ether was added dropwise 64 g of 4-carbethoxy-3,5-dimethylisoxazole in 100 ml of ether at a rate so that gentle reflux occurred. The addition was complete in about two hours, and the mixture was stirred overnight under nitrogen. A saturated solution of sodium sulfate was added dropwise under nitrogen until the excess lithium aluminum hydride was decomposed. The resulting suspension was filtered and the filtrate concentrated to an oil which was distilled to give 36.4 g of 3,5-dimethyl-4-hydroxymethylisoxazole, b.p. 130°-140° C. (0.1 mm).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05002960 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-216dd9ccd641402aab34f64cd3767c27 |
| 出典メモ | uspto-grants-1991_03 |