참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | (4-Aminophenoxy)benzene | HCID 8764 | — |
| 반응물 | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| 용매 | Dichloromethane methanol | HCID 21226129 | — |
| 생성물 | 1-(3-Phenoxyanilino)-4-(4-pyridylmethyl)phthalazine | HCID 22742003 | — |
반응 단계
A mixture of 256 mg (1.00 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 556 mg (3.00 mmol) 4-phenoxyaniline (Aldrich) is heated for 2 h at 90° C. The melt is cooled and stirred with 6 ml NH3 solution (10% in water: or 10 ml sat. NaHCO3 solution) and 15 ml dichloromethane/methanol 50:1 for 30 min. The aqueous phase is then separated off and extracted again with dichloromethane. The organic phase is dried (Na2SO4), concentrated by evaporation, and chromatographed (SiO2; ethyl acetate→ethyl acetate/CH3OH 19:1→10:1). Crystallization from acetonitrile yields the title compound: m.p.: 186-1 89° C.; Anal. calc. (C26H21N4O) C 77.02%, H 5.22%, N 13.82%; found C 77.2%, H 4.9%, N 13.8%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06258812B1 |
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| 출처 데이터셋 | uspto-grants-2001_07 |
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| ORD ID | ord-e4af79b0d7b34a93a608936e1f118b90 |
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| 출처 메모 | uspto-grants-2001_07 |
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