関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 152111 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-(Hydroxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 11137577 | — |
反応手順
Next, this methoxy methylene Meldrum's acid (25 g, 0.13 mol) was dissolved in chloroform (200 ml), followed by adding 2N-HCl (50 ml), agitating the mixture at room temperature, allowing it to still standing, separating the chloroform layer, saturating the aqueous layer with sodium chloride, extracting the solution with chloroform, combining the extract solution with the previously obtained chloroform solution, drying over anhydrous magnesium sulfate, filtering off the drying agent, and distilling off chloroform under reduced pressure to obtain raw formyl Meldrum's acid as residue, adding ether thereto, filtering off, further washing with ether, vaporizing the remaining ether and recrystallizing the resulting crystals from a mixed solvent of dichloromethanehexane to obtain formyl Meldrum's acid in the form of colorless crystals (20.5 g, yield 89%) having a m.p. of 95°-96° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04612379 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-941a64c8e984445f94afd9a75747a628 |
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| 出典メモ | uspto-grants-1986_09 |
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