関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Terephthalaldehyde | HCID 12173 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-(Diethylphosphoryl)-propionitrile | HCID 15917077 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Methyl-3-(4-formylphenyl)-2-propenonitrile | HCID 54558030 | 20.5% |
反応手順
360 g of a 30% solution of sodium methylate in methanol are added dropwise to a suspension of 134 g of terephthalaldehyde in 500 ml of methanol at 20°-25° C. 191 g of 2-(diethylphosphoryl)-propionitrile [prepared by the method of M. L. Raggio and D. S. Watt, J. Org. Chem. 41, 1873 (1976)] are now slowly added dropwise to the resulting reaction solution at 20°-25° C. The reaction mixture is stirred at room temperature for 6 hours and then poured onto 1,000 ml of water, and the aqueous suspension is adjusted to a pH value of 7 with acetic acid. The product which has precipitated is filtered off, dried and then chromatographed on silica gel. 35 g (20.5% of theory) of 2-methyl-3-(4-formylphenyl)-2-propenonitrile of the formula ##STR32## and then obtained in the form of colourless crystals having a melting point of 63°-64° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04346016 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-2ceca3f7db644803b0100fe27256f864 |
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| 出典メモ | uspto-grants-1982_08 |
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