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Diethyl Ether → 2,2-Dimethyl-1,3-dioxan-5-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,2-Dimethyl-1,3-dioxan-5-one | HCID 2733141 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2-Dimethyl-1,3-dioxan-5-ol | HCID 11029884 | 93.4% |
反応手順
To a diethyl ether (150 ml) solution of 2,2-dimethyl-1,3-dioxan-5-one (15 g, 0.115 mol), lithium aluminum hydride (4.38 g, 0.115 mol) was added at 0 to 8° C. for one hour in a nitrogen atmosphere. To the reaction mixture, water (4.2 ml), a 5N aqueous sodium hydroxide solution (4.2 ml), and water (12.8 ml) were sequentially added dropwise at 0 to 10° C. The mixture was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to obtain the title compound (14.2 g, 93.4%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425634B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-b7f23c757586434598dcb08ac7ddb4a1 |
| 出典メモ | uspto-grants-2008_09 |