関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | Hydrogenated cardanol | HCID 68146 | — |
| 反応物 | 1,2-Benzenedicarbonitrile, 4-nitro- | HCID 97443 | — |
| 生成物 | 4-(3-Pentadecyl)phenoxyphthalonitrile | HCID 67501864 | 84% |
反応手順
To a 5 liter 1 necked round bottomed flask equipped with mechanical stirrer was added 502.5 grams (1.65 mole) of 3-pentadecylphenol, 200 grams (1.45 mole) of potassium carbonate, and 2,000 grams of 1-methyl-2-pyrrolidinone (anhydrous; obtained from Aldrich Chemical Co.). The mixture was heated to 90° C. for 2 hours using a heating mantle. The reaction mixture turned dark brown. Thereafter, 250.0 grams (1.45 mole) of 4-nitrophthalonitrile (obtained from Sigma-Aldrich) was added and the mixture was maintained at 90° C. for an additional 2 hours. The hot reaction mixture was then quenched by slowly pouring it into 3 liters of deionized water. The precipitated beige suspension was stirred until it had cooled to room temperature, then was filtered. The solid was then reslurried and filtered, using about 6 liter portions of deionized water, until the water used to wash the solid product was of neutral pH. The solid was then twice reslurried in 4 liters of methanol, filtered, and vacuum dried at 40° C. to give 519.8 grams (84 percent yield) of 4-(3-pentadecyl)phenoxyphthalonitrile. The purity of this material as measured by HPLC was more than 89 percent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06472523B1 |
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| 出典データセット | uspto-grants-2002_10 |
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| ORD ID | ord-703e9cc5c668471b89d340ed43938185 |
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| 出典メモ | uspto-grants-2002_10 |
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