関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Allyl bromide | HCID 7841 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Tetrabromoterephthalic Acid | HCID 224162 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Diallyl tetrabromoterephthalate | HCID 20223631 | — |
反応手順
To a liquid mixture consisting of 19.3 parts of tetrabromoterephthalic acid and 40 parts of isopropyl alcohol, were added with stirring 13 parts of a 50% aqueous solution of caustic potash. After continuously mixing the thus-obtained mixture for 30 minutes, 12.6 parts of allyl bromide and 1.0 part of triethylamine were added. The resulting mixture was heated until isopropanol started to reflux. The mixture was maintained at the temperature for 8 hours. After allowing the resulting reaction mixture to cool, the liquid reaction mixture was concentrated under reduced pressures, followed by an addition of 50 parts of chloroform to dissolve the residue. The resultant solution was poured in a separation funnel and then washed with an aqueous solution of sodium bicarbonate and thereafter with water. The organic layer was concentrated and the resultant white solid was recrystallized from ethyl acetate, thereby obtaining 12 parts of diallyl tetrabromoterephthalate (hereinafter called "Compound B") as white irregular crystals (m.p. 125°-127° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04522993 |
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| 出典データセット | uspto-grants-1985_06 |
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| ORD ID | ord-1b2a38301350493cbc10ef3a0c03e3dd |
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| 出典メモ | uspto-grants-1985_06 |
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