関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 2-Bromo-2'-acetonaphthone | HCID 69179 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 生成物 | 1,3-Dioxolane, 2-(bromomethyl)-2-(2-naphthalenyl)- | HCID 607997 | — |
反応手順
To a stirred solution of 74.4 parts of 2-bromo-1-(2-naphthalenyl)-1-ethanone in 240 parts of butanol are added successively 3 parts of 4-methylbenzenesulfonic acid and 270 parts of benzene. Then there are added dropwise 28 parts of 1,2-ethanediol. Upon completion, stirring is continued overnight at reflux temperature. The reaction mixture is evaporated. The residue is dissolved in 2,2'-oxybispropane and the solution is stirred with a diluted sodium hydroxide solution. The layers are separated and the aqueous phase is extracted with 2,2'-oxybispropane. The extract is neutralized with water, dried, filtered and evaporated. The oily residue is crystallized from methanol. The product is filtered off and recrystallized from methanol, yielding 41 parts of 2-(bromomethyl)-2-(2-naphthalenyl)-1,3-dioxolane; mp. 64° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04160838 |
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| 出典データセット | uspto-grants-1979_07 |
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| ORD ID | ord-0c516d00863c46ada44e4db8fd091834 |
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| 出典メモ | uspto-grants-1979_07 |
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