関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Hexadecyl methanesulfonate | HCID 519810 | — |
| 反応物 | (2-Phenyl-1,3-dioxan-5-yl)methanol | HCID 10679342 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 5-Hexadecyloxymethyl-2-phenyl-1,3-dioxane | HCID 19884202 | 97% |
反応手順
A suspension of 7.769 g (40 mM) of 5-hydroxymethyl-2-phenyl-1,3-dioxane n1 and 2.08 g (52 mM) of 60% sodium hydride in oil in 150 ml of anhydrous benzene is heated at 50° C. for 1 hour then a solution of 17.28 g (54 mM) of n-hexadecyl methanesulfonate in 50 ml of anhydrous benzene is added. The reaction mixture is heated under refluxing for 7 hours. The product is isolated by ethyl acetate extraction. The ethyl acetate layer is washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and evaporated. Crystallization of the residue from n-pentane-methanol affords 16.203 g (97% yield) of the titled compound n2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05047540 |
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| 出典データセット | uspto-grants-1991_09 |
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| ORD ID | ord-77066b4b4e9243eaa30cff8652522946 |
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| 出典メモ | uspto-grants-1991_09 |
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