참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 3-Methyl-5-(tributylstannyl)isoxazole | HCID 2763255 | — |
| 반응물 | 5-Chloro-2,3-difluoropyridine | HCID 2783248 | — |
| 반응물 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 생성물 | 2,3-Difluoro-5-(3-methylisoxazol-5-yl)pyridine | HCID 58015534 | 55.4% |
반응 단계
A 330 mL pressure vessel was charged with 5-chloro-2,3-difluoropyridine (5.00 g, 33.4 mmol), 3-methyl-5-(tributylstannyl)isoxazole (14.9 g, 40.1 mmol), XPhos (2.23 g, 4.68 mmol), PdOAc2 (0.526 g, 2.34 mmol), and 1,4-dioxane (167 ml, 33.4 mmol), flushed with argon, sealed, then heated at 100° C. for 16 hours. The mixture was concentrated; the black oil was absorbed onto silica gel and purified by MPLC, eluting with 20% EtOAc in hexanes isocratic to yield an orange solid; this was triturated with hexanes to give 2,3-difluoro-5-(3-methylisoxazol-5-yl)pyridine (3.6278 g, 55.3% yield) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08198448B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-cb12bebbeccc4a719bb91e95332a4562 |
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| 출처 메모 | uspto-grants-2012_06 |
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