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p-Toluenesulfonic acid → 1,10-Phenanthroline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1,10-Phenanthrolin-5-amine | HCID 606970 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,10-Phenanthroline | HCID 1318 | 85% |
反応手順
3.05 mM of the 4-di(2-thienyl)-1,4-butanedione obtained from Step 1 described above, 3.03 mM of 1,10-phenanthroline-5-amine, and 5.4 mM of p-toluene sulfonic acid were dissolved in toluene, and then refluxed under a nitrogen current for 4 days. The refluxed mixture was cooled to room temperature, and then toluene was removed from the mixture. The remaining material was dissolved in 5 ml of 99.8% dichloromethane solution, and eluted by using a silica column to obtain 5-di(thiophen-2-yl)-1H-pyrrol-1-yl)-1,10-phenanthroline. The yield was 85%, and the structure was confirmed by using 1H NMR. The spectroscopic data thereof is as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09175328B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-a610498926d4441ebcb1a453dfd1a538 |
| 出典メモ | uspto-grants-2015_11 |