関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | N,N'-Diphenyl-P-Phenylenediamine | HCID 6319 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Nitrobenzene | HCID 7416 | — |
| 生成物 | 1,4-Benzenediamine, N1,N1,N4,N4-tetraphenyl- | HCID 84207 | 111.3% |
反応手順
41.4 g of N,N′-diphenyl-p-phenylenediamine, 66 g of iodobenzene, 100 ml of nitrobenzene, 45 g of K2CO3, 10.8 g of copper powder, and I2 (trace) were put in a four-neck flask of 300-milliliter volume, and were refluxed gently over 24 hours by stirring the same while removing generated water by reflux. Subsequently, steam distillation was carried out, and when a distillate no longer came out, residues were filtered out after cooling, washed with water, and extracted using toluene. After removing toluene by distillation, ethanol was added to the residues, and the mixture was filtered. Recrystallization was carried out using a solvent of toluene and ethanol (toluene:ethanol=4:1 (by volume)), whereby 36.5 g of N,N,N′,N′-tetraphenyl-p-phenylenediamine was obtained. It had a melting point of 200° C. to 202° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07083863B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-77814c110edc4862859dc162723022c7 |
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| 出典メモ | uspto-grants-2006_08 |
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