참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | P-Phenylenediamine | HCID 7814 | — |
| 반응물 | 1-Chloro-4-phenylphthalazine | HCID 272109 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 57756220 | HCID 57756220 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07560551B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-6075b051e6e9493d9a18c6d2569faf92 |
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| 출처 메모 | uspto-grants-2009_07 |
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