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Water → 2-(3-Hydroxypropyl)-2-phenyl-1,3-dioxolane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-[2-(Methoxycarbonyl)ethyl]-2-phenyl-1,3-dioxolane | HCID 10037102 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(3-Hydroxypropyl)-2-phenyl-1,3-dioxolane | HCID 22344557 | 87% |
反応手順
A solution of 2-[2-(methoxycarbonyl)ethyl]-2-phenyl-1,3-dioxolane (5.00 g) in diethyl ether (15 ml) was added dropwise to a mixture of lithium aluminium hydride (949 mg) and diethyl ether (30 ml) at 0° C. After stirring for 30 minutes, water was added to the reaction mixture carefully and the precipitates were removed by filtration. The filtrate was extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous saturated solution of sodium chloride, dried (MgSO4) and concentrated. The residue was subjected to silica gel chromatography to obtain 2-(3-hydroxypropyl)-2-phenyl-1,3-dioxolane (3.81 g, yield 87%) as a colorless oil from an ethyl acetate-hexane (2:3, v/v)-eluted fraction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06924300B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-619da3d6a42a4cb78beec7dd117f318e |
| 出典メモ | uspto-grants-2005_08 |