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p-Toluenesulfonic acid → 4,4'-Dibromotriphenylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1,4-Cyclohexanedione | HCID 12511 | — |
| 反応物 | Bis(4-bromophenyl)amine | HCID 629950 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4,4'-Dibromotriphenylamine | HCID 13594707 | 67% |
反応手順
A mixture of 4,4′-dibromodiphenylamine (7.3 g. 22 mmol), cyclohexane-1,4-dione (2.5 g., 23.3 mole), para-toluenesulfonic acid (0.1 g.), and toluene (100 mL) was kept at reflux with a Dean-Stark 15 phase separator containing 4A molecular sieves. After 18 hours at reflux, the reaction was diluted with toluene, and the toluene solution was washed with water, dried, and concentrated. The residue was dissolved in hexanes, and the hexanes solution was then passed through a column of silica gel to afford 4,4′-dibromotriphenylamine as a colorless glass, 5.04 g., 67% yield. Mass Spec (m/z): 401, 403, 405 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09024037B1 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-bdf96a7afd554b108fcf9d56789309d2 |
| 出典メモ | uspto-grants-2015_05 |