참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzylamine | HCID 7504 | — |
| 반응물 | 3-Chloro-6-methylpyridazine | HCID 227254 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Dichloro[1,1'-bis(di-tert-butylphosphino)ferrocene]palladium(II) | HCID 53384307 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | N-benzyl-6-methylpyridazin-3-amine | HCID 61313509 | 91.3% |
반응 단계
To a stirred solution of 3-chloro-6-methylpyridazine (215 mg, 1.66 mmol) and benzylamine (267 mg, 2.5 mmol) in toluene (20 mL) was added sodium tert-butoxide (480 mg, 5.0 mmol) and [1,1′-bis(di-tert-butylphosphino)ferrocene]palladium(II) dichloride (20 mg). The reaction mixture was stirred at 140° C. under microwave irradiation for 2 h, then cooled to room temperature and concentrated in vacuo. The residue was purified by column chromatography (SiO2, 0-100% EtOAc/heptane) to give the title compound (302 mg, 91%) as an off-white solid. δH (CDCl3) 7.25-7.41 (5H, m), 7.02 (1H, d, J 9.0 Hz), 6.55 (1H, d, J 9.0 Hz), 4.91 (1H, s), 4.60 (2H, d, J 5.8 Hz), 2.53 (3H, s). LCMS (ES+) 200 (M+H)+, RT 2.50 minutes (Method 2).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08242116B2 |
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| 출처 데이터셋 | uspto-grants-2012_08 |
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| ORD ID | ord-97edd6a3912e4bb496eba53b2e8f2b55 |
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| 출처 메모 | uspto-grants-2012_08 |
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