関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,4'-Dihydroxybiphenyl | HCID 7112 | — |
| 反応物 | 1,3-Dinitrobenzene | HCID 7452 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4,4'-Bis(3-nitrophenoxy)biphenyl | HCID 6611814 | 99.5% |
反応手順
A 3 liter glass reaction vessel was charged with 186 grams (1.0 mol) of 4,4'-dihydroxybiphenyl, 438 grams (2.6 mols) of m-dinitrobenzene, 363 grams of potassium carbonate and 2,000 ml of N,N-dimethylformamide. The mixture was reacted at a temperature of 145°-150° C. for 16 hours. After completing the reaction, the resultant mixture was cooled and filtered to remove potassium nitrite. The solvent was distilled off from the filtrate under reduced pressure. The residue was cooled to 65° C., added with 2,000 ml of methanol and stirred for an hour. The resulted crystals were filtered, washed with water, washed with methanol and dried to obtain 426 grams (99.5% yield) of 4,4'-bis(3-nitrophenoxy)biphenyl as brown crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04847311 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-ce659955b949483983e33552a15ad669 |
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| 出典メモ | uspto-grants-1989_07 |
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