反応式
CN1Cc2ccc(Cl)nc2O[C@H](c2ccccc2)C1.COc1nc(N)ccc1-c1cnn(C)c1>CC(=O)O.CC(=O)O.Cc1ccccc1.O=C([O-])[O-].[K+].[K+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>COc1nc(Nc2ccc3c(n2)O[C@H](c2ccccc2)CN(C)C3)ccc1-c1cnn(C)c1参加物
反応物 2
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 110 °C
実験手順
Charged a round-bottom flask with a mixture of 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (0.76 g, 3.72 mmol), (R)-8-chloro-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (1.022 g, 3.72 mmol), palladium (II) acetate (0.025 g, 0.11 mmol), rac-BINAP (0.116 g, 0.19 mmol), potassium carbonate (0.926 g, 6.70 mmol), and toluene (15 mL). The atmosphere was inerted through consecutive vacuum-nitrogen purge cycles, then heated at 110 °C under N2(g) for 16 hours. HPLC-UV shows a small percentage (3-6% depending on wavelength) of oxazepine remaining, aminopyridine if fully converted. The mixture was allowed to cool to room temperature. DCM and 2M HCl was added and the orgaic phase were removed. The aqueous phase were basified using solid KOH and a 4M solution. Extracted with DCM, dried oved MgSO4 and concentrated.
出典と根拠
- ORDレコード
- ord-d106e5c0510845f092f0e721b9abc1a2
- 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
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