関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Ethyl acetoacetate ethyleneglycol ketal | HCID 80865 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1,3-Dioxolane-2-ethanol, 2-methyl- | HCID 538382 | 98.8% |
反応手順
Lithium aluminium hydride (2 g, 51 mmol) is added in small portions to anhydrous ethyl ether (200 cc). The mixture is cooled to 0° C. and ethyl 3,3-ethylenedioxybutanoate (3 g, 17 mmol) is then added over 10 minutes as a solution in anhydrous ethyl ether (10 cc). The mixture is stirred for 2 hours 30 minutes at a temperature in the region of 20° C. and is then hydrolysed by adding a saturated sodium sulphate solution (12 cc). After 2 hours the white precipitate is separated off by filtration. The organic phases are dried over magnesium sulphate. 2,2-Ethylenedioxy-4-hydroxybutane (2.22 g) is thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04876370 |
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| 出典データセット | uspto-grants-1989_10 |
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| ORD ID | ord-786108f8e0884391b91fb34e5c910ad8 |
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| 出典メモ | uspto-grants-1989_10 |
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