関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1,3-Dioxolane | HCID 12586 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Tetradecylphenol | HCID 116800 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-(4-Tetradecylphenoxy)-1,2-propanediol | HCID 20219899 | — |
反応手順
An about 43.5 g portion of 4-tetradecyl phenol was added in portions to a suspension of about 10.8 g of prewashed sodium hydride in dimethylformamide. The mixture was refluxed about 11/2 hours, allowed to cool and about 37.8 g of 2,2-dimethyl-4-[[methylsulfonyl)oxy]methyl]-1,3-dioxolane was added. This mixture was heated to about 80° C. for about 24 hours; diluted with hexane and ether, washed with water and brine and evaporated. The residue was heated on a steam bath with about 500 ml of methanol and about 80 ml of dilute hydrochloric acid for one hour, cooled, partially evaporated, the solid collected and recrystallized from methanol, giving about 38 g of the desired title compound, mp 81.5°-83.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04640913 |
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| 出典データセット | uspto-grants-1987_02 |
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| ORD ID | ord-65c54c27b3da49ca840c4785aa94538a |
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| 出典メモ | uspto-grants-1987_02 |
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