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 a 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 extra ct 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 | US04079062 |
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| 出典データセット | uspto-grants-1978_03 |
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| ORD ID | ord-4c3488e9e9b24c9492349b3290d13e59 |
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| 出典メモ | uspto-grants-1978_03 |
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