関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Epichlorohydrin | HCID 7835 | — |
| 反応物 | 4-Phenoxyphenol | HCID 13254 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-phenoxy-O-(2-hydroxy-3-chloropropyl)phenol | HCID 22247712 | — |
反応手順
A four-neck flask equipped with a thermometer, dropping funnel, condenser tube and stirrer was charged with 305.3 g (3.3 mol) of epichlorohydrin, and while nitrogen purging was performed, the temperature was raised to 70° C. Into the flask, 204.8 g (1.1 mol) of 4-phenoxyphenol dissolved in 1020 g of ethanol was added dropwise taking 4 hours. Further, stirring was performed for 6 hours, to complete the addition reaction, for obtaining 4-phenoxy-O-(2-hydroxy-3-chloropropyl)phenol. In succession, the temperature in the flask was lowered to 25° C., and into the flask, 229 g (2.75 mol) of 48% NaOH aqueous solution was added dropwise taking 2 hours. Further, stirring was performed for 1 hour. After completion of cyclization reaction, ethanol was distilled away, and 410 g of toluene was used for extraction, 5% saline solution being used for washing twice. Toluene and epichlorohydrin were removed from the organic layer under reduced pressure, to obtain 215.6 g of a viscous liquid (yield 89%). The purity of 4-phenoxyphenyl glycidyl ether as the main product was 92% (GCarea %).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434811B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-08902dd1257f4b6f9ee352acd169a027 |
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| 出典メモ | uspto-grants-2016_09 |
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