反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 95 °C
PROCEDURE
实验过程
A 50 mL round-bottomed flask equipped with a reflux condenser was charged with 101b (500 mg, 1.14 mmol), [4-(dihydroxyboranyl)-2-{4,4-dimethyl-9-oxo-1,10-diazatricyclo[6.4.0.02,6]dodeca-2(6),7-dien-10-yl}pyridin-3-yl]methyl acetate 101c (452 mg, 1.14 mmol), K3PO4 (483 mg, 2.28 mmol), NaOAc (187 mg, 2.28 mmol), Pd(dppf)Cl2 (42 mg, 0.057 mmol), and CH3CN/H2O (20.0/0.5 mL). The system was subject to three cycles of vacuum/argon flush then heated at 95° C. under N2 for 1 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The residue was purified by silica-gel column-chromatography eluting with DCM/MeOH (70:1 to 30:1) to afford 101d (400 mg, 50%) as yellow solid. MS-ESI: [M+H]+ 712.3
WORKUP
后处理
- customA 50 mL round-bottomed flask equipped with a reflux condenser
- customflush
- temperatureThe reaction mixture was cooled to room temperature
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica-gel column-chromatography
- washeluting with DCM/MeOH (70:1 to 30:1)