참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Methylpiperazine | HCID 53167 | — |
| 반응물 | 2-Chloro-4-iodopyridine | HCID 1516511 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Dichloro[1,1'-bis(di-tert-butylphosphino)ferrocene]palladium(II) | HCID 53384307 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-(2-Chloropyridin-4-YL)-4-methylpiperazine | HCID 72218899 | 77% |
반응 단계
To a mixture of 2-chloro-4-iodopyridine (300 mg, 1.24 mmol) in toluene (4 mL) was added 1-methylpiperazine (0.14 mL, 1.24 mmol), sodium tert-butoxide (239 mg, 2.44 mmol), [1,1′-bis(di-tert-butylphosphino)ferrocene]palladium(II) dichloride (30 mg, 10% wt) and the suspension was heated to 115° C. under microwave irradiation for 30 minutes. The resulting mixture was concentrated in vacuo and partitioned between DCM (50 mL) and water (50 mL). The organic phase was washed with brine (50 mL), dried (MgSO4), and evaporated in vacuo to give the title compound (200 mg, 77%) as a brown oil. LCMS (ES+) 212.0 (M+H)+, RT 1.78 minutes (70% purity) (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-36642310d6664144b76b5f68ff44f51e |
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| 출처 메모 | uspto-grants-2012_08 |
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