関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoic Acid | HCID 243 | — |
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Allyl methacrylate | HCID 7274 | — |
| 反応物 | Lauryl Methacrylate | HCID 8906 | — |
| 反応物 | 4-Vinylbenzoic acid | HCID 14098 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Vinylbenzoic acid | HCID 3015504 | — |
反応手順
Into a 500 ml. 2-necked flask fitted with a thermometer, and a reflux condenser connected to a N2 source, was introduced a mixture of 3.5 g of 4-vinylbenzoic acid (Aldrich Chemical Co. , 3 g of allyl methacrylate, 150 ml tetrahydrofuran and 150 ml ethylacetate. The mixture was stirred to dissolve the benzoic acid compound. Next was added 93.5 g of laurylmethacrylate. The flask was purged with N2 and heated at 70° C. for 10 minutes. The flask was purged again with N2 and 1 g of 2,2-azobisisobutyronitrile (AIBN) was added all at once and heated at 70° C. under a N2 blanket. This was continued for a period of 8 hours. The resulting polymeric solution was cooled to room temperature and diluted with twice its volume with Isopar™ G and filtered to remove insoluble materials (About 125 mg of homopolymer of VBA acid remained on the filter paper). The clear filtered polymeric solution was further diluted with Isopar™ G to 4.1 liters and was subjected to distillation under reduced pressure until about 500 ml of the distillate was collected in the receiving flask. The distillate was mainly ethylacetate, tetrahydrofuran and Isopar™ G).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05066559 |
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| 出典データセット | uspto-grants-1991_11 |
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| ORD ID | ord-f4a56db9433e4313ac9b26d3334542cb |
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| 出典メモ | uspto-grants-1991_11 |
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