참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Bromopyridinium chloride | HCID 88100 | — |
| 반응물 | Pyridazine, 3-phenyl-5-(tributylstannyl)- | HCID 11729979 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ammonium Chloride | HCID 25517 | — |
| 생성물 | Pyridazine, 3-phenyl-5-(4-pyridinyl)- | HCID 10198553 | 69.4% |
반응 단계
3-Phenyl-5-(tri-n-butylstannyl)pyridazine (110 mg, 0.247 mmol), 4-bromopyridine hydrochloride (72 mg, 0.370 mmol) and Pd(PPh3)4 (10 mg) in THF (2 ml) were combined and heated to 150° C. for 60 min in a Smith Synthesiser microwave reactor (Personal Chemistry, Uppsala, Sweden). The reaction was diluted with CH2Cl2 (6 ml) and NH4Cl (2 ml) then poured into PTFE (5 μM) fritted syringe barrels. The organic phase was collected and concentrated while loading onto silica. The compound was purified by dry flash column chromatography to give the title compound as a white solid (40 mg). δH (400 MHz, d6 DMSO) 7.36-7.63 (3H, m), 8.10 (2H, dd, J 1.8 and 4.5), 8.32 (2H, m), 8.62 (1H, d, J 2.0), 8.80-8.82 (2H, dd, J 1.8 and 4.5), 9.71 (2H, d, J 2.0); m/z (ES+) 234 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07381725B2 |
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| 출처 데이터셋 | uspto-grants-2008_06 |
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| ORD ID | ord-6ab7387de01244b79f01f726fa6820c7 |
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| 출처 메모 | uspto-grants-2008_06 |
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