関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | P-Phenylenediamine | HCID 7814 | — |
| 反応物 | 1-Chloro-4-phenylphthalazine | HCID 272109 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 57756220 | HCID 57756220 | — |
反応手順
Benzene-1,4-diamine (0.337 g, 3.12 mmol) and 1-chloro-4-phenylphthalazine (0.500 g, 2.08 mmol) were treated with 7.5 mL 2-BuOH in a sealed tube and heated to 110° C. The reaction quickly became a solid, yellow mass. After several hours, the reaction was cooled and diluted with water. The slurry was then partitioned between DCM and 1N NaOH. The aqueous layer was extracted into DCM (2×). The combined organic layers were dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The resulting material was purified by silica gel chromatography, ISCO, 40 g, 0-10% MeOH/MC to give N1-(4-phenylphthalazin-1-yl)benzene-1,4-diamine as an orange-brown solid. MS m/z=313 [M+H]+. Calc'd for C20H16N4: 312.4.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560551B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-6075b051e6e9493d9a18c6d2569faf92 |
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| 出典メモ | uspto-grants-2009_07 |
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