関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Terephthalaldehyde | HCID 12173 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Diethyl (4-Cyanobenzyl)phosphonate | HCID 241438 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Cyanostilbene-4'-aldehyde | HCID 54138187 | 91% |
反応手順
With stirring, cooling and blanketing with nitrogen, 6.7 g of terephthalaldehyde are added in portions to a mixture of 6.2 ml of aqueous potassium hydroxide solution 50% w/v and 40 ml of methanol, such that the temperature does not exceed 22° C. The resultant solution is then treated dropwise at 10° C. over 1/2 hour with a solution of 12.7 g of p-diethylphosphonomethylbenzonitrile (99.5%) in 10 ml of methanol, whereupon the reaction product soon precipitates. After stirring overnight at 10° C., the thick suspension is neutralised with 3 ml of glacial acetic acid, diluted with 40 ml of water, and filtered with suction. The filter residue is washed repeatedly with a 3:2 mixture of methanol/water and then with water until salt-free and dried under vacuum at 80° C., affording 10.6 g of 4-cyanostilbene-4'-aldehyde as a pale yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04778622 |
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| 出典データセット | uspto-grants-1988_10 |
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| ORD ID | ord-440b588564de4ffba647310ad7ef0456 |
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| 出典メモ | uspto-grants-1988_10 |
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