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Ethylene Glycol → 2-[2-(Methoxycarbonyl)ethyl]-2-phenyl-1,3-dioxolane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Benzenebutanoic acid, gamma-oxo-, methyl ester | HCID 141190 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-[2-(Methoxycarbonyl)ethyl]-2-phenyl-1,3-dioxolane | HCID 10037102 | — |
反応手順
To a solution of 2.0 g of 3-benzoylpropionic acid methyl ester in 50 ml of dry benzene were added 0.7 ml of ethylene glycol and 0.01 g of anhydrous-p-toluene-sulfonic acid and the mixture was heated under reflux for 17 hours while removing water formed during the reaction by using a molecular sieve. After cooling, the reaction mixture was washed with a saturated sodium chloride aqueous solution, and concentrated under reduced pressure. The residue was purified by silica gel flash column chromatography (eluent: benzene/hexane=1/1 by volume) to obtain 1.8 g of 4,4-ethylenedioxy-4-phenylbutyric acid methyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04863904 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-17cb79a884504a5682a49f850efe5a25 |
| 出典メモ | uspto-grants-1989_09 |