関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Benzyl Chloride | HCID 7503 | — |
| 反応物 | Solketal | HCID 7528 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,2-Dimethyl-4-((phenylmethoxy)methyl)-1,3-dioxolane | HCID 85795 | — |
反応手順
To a 1000 ml round-bottom flask fitted with a thermometer, a nitrogen-introducing tube, and a stirrer were added 132.2 g (1.0 mol) of 2,2-dimethyl-1,3-dioxolane-4-methanol, 202.5 g (1.05 mol) of a 28% methanol solution of sodium methoxide, and 600 ml of toluene. With introducing nitrogen thereinto, the toluene was refluxed under reduced pressure for 1 hour to remove the methanol by distillation. With maintaining the solution at 80° C., 126.6 g (1.0 mol) of benzyl chloride was added dropwise over a period of 2 hours using a dropping funnel, followed by further 2 hours of reaction. After completion of the reaction, the temperature was lowered to 60° C. and 10 g of KYOWAAD 600 was added thereto, followed by 1 hour of stirring. The reaction liquid was filtrated, the solvent was removed, and the residue was purified by distillation (b.p. 93-95° C./266 Pa) to obtain 4-(benzyloxymethyl)-2,2-dimethyl-1,3-dioxolane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08828373B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-04875b4527034c489320265dac7e0f76 |
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| 出典メモ | uspto-grants-2014_09 |
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