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1-Iodonaphthalene → N,N-Bis(3,4-dimethylphenyl)naphthalen-1-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Iodonaphthalene | HCID 7004 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Bis(3,4-dimethylphenyl)amine | HCID 614511 | — |
| 触媒 | Copper sulfate pentahydrate | HCID 24463 | — |
| 溶媒 | Tridecane | HCID 12388 | — |
| 生成物 | N,N-Bis(3,4-dimethylphenyl)naphthalen-1-amine | HCID 23362688 | 37.4% |
反応手順
In 100-ml three-neck flask were placed 7.2 g of 3,3',4,4'-tetramethyldiphenylamine synthesized in Example 3 (1), 12.2 g of 1-iodonaphthalene, 5 g of anhydrous potassium carbonate, 0.5 g of copper sulfate pentahydrate and 10 ml of n-tridecane, and after carrying out the reaction for 25 hours at 200° C. under a nitrogen gas atmosphere, the reaction mixture was cooled to room temperature. The reaction mixture was subjected to a column purification (solvent: n-hexane) with activated alumina and the solvent was distilled under reduced pressure. The residue was recrystallized from ethanol to provide 4.2 g of N,N-bis(3,4-dimethylphenyl)naphthalene-1-amine. (Melting point 125° to 127° C., light yellow crystals, IR spectrum shown in FIG. 5.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05495049 |
| 出典データセット | uspto-grants-1996_02 |
| ORD ID | ord-649938a754044e90a20de6e4130055bc |
| 出典メモ | uspto-grants-1996_02 |