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Sodium Hydroxide → 2,2-Difluoro-5-methoxy-1-pentanal oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Hydroxylamine, N-chloro- | HCID 149953 | — |
| 反応物 | 2,2-Difluoro-5-methoxy-1-pentanal hydrate | HCID 20149453 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 2,2-Difluoro-5-methoxy-1-pentanal oxime | HCID 73664053 | 91% |
反応手順
A mixture of 2,2-difluoro-5-methoxy-1-pentanal hydrate (1.57 g, 9.2 mmoles), hydroxylamino hydrochloride (640 mg, 9.2 mmoles), 1N NaOH (9.2 ml), and dioxane (15 ml) is kept for 1 hour at room temperature. After addition of ether and brine, usual extraction gives an oil which according to NMR is the oxime hydrate. Several evaporations with carbon tetrachloride (50° C., 60 mm Hg) afford the oxime (1.4 g) which is purified by chromatography on silica (ethyl acetate/petroleum ether: 20/80, RF: 0.53): 1.05 g (68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04730006 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-cdffc9b431c346c79072bd402f130673 |
| 出典メモ | uspto-grants-1988_03 |