関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Furan | HCID 8029 | — |
| 触媒 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | Methyl Acrylate | HCID 7294 | 292.2% |
| 生成物 | Methyl 7-oxabicyclo[2.2.1]hept-5-ene-2-carboxylate | HCID 12271748 | — |
反応手順
1290 g (15 Mol) methylacrylate is prepared and 67.5 g (0.5 Mol) AlCl3 added thereto and dissolved with stirring. At 20° to 25° C., 1050 g (15.4 Mol) furane is added drop-wise during cooling. The temperature is maintained at 20° C. until the exothermic reaction is finished, after which stirring is continued for a further hour at 20° C. and then for 3 hours at 10° C. 300 g water is then added, the organic phase separated, and the unconverted furane and the methylacrylate distilled off under a pressure of 10 Torr and at a bath temperature of 60° C. in a rotary evaporator. Finally, the vacuum is lowered to 1 Torr and further volatile components drawn off. The crude product is passed to a thin-film evaporator under a vacuum of 1 Torr and a thermostatically controlled temperature of 95° C. A distillation temperature of approximately 70° C. is used. The 2-carbomethoxy-7-oxabicyclo(2,2,1)hept-5-ene is obtained in a yield of 1060 g (45.9% theoretical).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04555581 |
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| 出典データセット | uspto-grants-1985_11 |
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| ORD ID | ord-a289d304ea744587904277b0d0f30caa |
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| 出典メモ | uspto-grants-1985_11 |
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