関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | 4-Iodotoluene | HCID 12207 | — |
| 反応物 | 1,5-Diaminonaphthalene | HCID 16720 | — |
| 反応物 | 1,5-Bis(phenylamino)naphthalene | HCID 229939 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,5-bis(Phenyl-p-tolylamino)naphthalene | HCID 18411142 | — |
反応手順
8 gram (0.05 mol) of 1,5-diamino naphthalene, 22 gram (0.11 mol) of iodobenzene, 17 gram (0.12 mol) of potassium carbonate, 0.4 gram of copper powder and 50 milliliter of nitrobenzene were introduced in a 100 milliliter three-necked flask for stirring at 200° C. for 30 hours. After the reaction, toluene was added, followed by filtration for removal of inorganic compounds. Toluene and nitrobenzene were removed by distillation in a reduced pressure ambient, and the remainder was subjected to separation refinement in a silica gel column using a 1:3 mixture solvent of toluene and ligroin, to prepare 10 gram of 1,5-bis(phenylamino)naphthalene. Thereafter, 6.2 gram (0.02 mol) of 1,5-bis(phenylamino)naphthalene, 11 gram (0.05 mol) of p-iodotoluene, 7 gram (0.05 mol) of potassium carbonate, 0.3 gram of copper powder and 50 milliliter of nitrobenzene were introduced in a 100 milliliter three-necked flask for stirring at 200° C. for 30 hours. After the reaction, toluene was added, followed by filtration for removal of inorganic compounds. Toluene and nitrobenzene were removed by distillation in a reduced pressure ambient, and the remainder was subjected to separation refinement in a silica gel column using a 1:3 mixture solvent of toluene and ligroin, to prepare 7 gram of 1,5-bis(phenyl-p-tolylamino)naphthalene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06468675B1 |
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| 出典データセット | uspto-grants-2002_10 |
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| ORD ID | ord-ffdd0ddee9ae40e1a80bf09ab9ee792c |
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| 出典メモ | uspto-grants-2002_10 |
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