반응식
Fc1ccc(Br)c(Cl)c1.O=C1CCNCC1>CC(=O)O.CC(=O)O.CC(C)(C)[O-].CC(C)c1cc(C(C)C)c(-c2ccccc2P(C2CCCCC2)C2CCCCC2)c(C(C)C)c1.Cc1ccccc1.[Na+].[Pd]>O=C1CCN(c2ccc(F)cc2Cl)CC1참가 물질
반응물 2
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 120 °C
실험 절차
To a round bottom flask was added palladium(II) acetate (0.012 g, 0.06 mmol), dicyclohexyl(2',4',6'-triisopropylbiphenyl-2-yl)phosphine (0.026 g, 0.06 mmol), and sodium tert-butoxide (0.213 g, 2.21 mmol). Added 5 mL toluene/t-butanol mix and purged with nitrogen. Added piperidin-4-one (0.15 g, 1.11 mmol), in 3 mL tol/tbuoh (slurry), followed by 1-bromo-2-chloro-4-fluorobenzene (0.255 g, 1.22 mmol), in 2 mL tol/tbuoh. Flushed with additional nitrogen and then heated to 120oC overnight. Let reaction mixture cool to room temperature and filtered through Celite. Rinsed repeatedly with EtOAc and concentrated in vacuo. Purified via ISCO 12g SiO2 column using 0-20% hexanes/ethyl acetate. Fractions 19 and 20 were combined and concentrated to afford a white solid. NMR (I200805922.42) shows a mess. Discarded. Will try another way.
출처 및 근거
- ORD 기록
- ord-5c5d7fac90d14102bcad7fe6bdad56a8
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
연결된 노트
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