反応式
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)CC1参加物
反応物 2
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 120 °C
実験手順
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.
出典と根拠
- ORDレコード
- ord-5c5d7fac90d14102bcad7fe6bdad56a8
- 出典データセット
- 750 AstraZeneca ELN dataset
- 元リンク
- 出典を表示
関連ノート
読み込み中…