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Sodium Acetate → 2,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl- | HCID 11816152 | — |
| 反応物 | HCID 178418287 | HCID 178418287 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane | HCID 12012816 | 92% |
反応手順
2,2-Dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane (33 g.) was added to a stirred suspension of pyridinium chlorochromate (122.6 g) and anhydrous sodium acetate (7.8 g.) in dry dichloromethane (200 ml.), at 0°, under a current of nitrogen. The mixture was stirred at room temperature for six hours. The mixture was diluted with dry ether (500 ml) and the organic solution was decanted off. The oily residue was treated with ether and the combined extracts were evaporated in vacuo. The residue was purified by chromatography on silica, eluting with ether: hexane 1:3. 2,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane (30 g.) was obtained as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04985582 |
| 出典データセット | uspto-grants-1991_01 |
| ORD ID | ord-7ab9d0024105477a8aa63b1591117185 |
| 出典メモ | uspto-grants-1991_01 |