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
- 80 °C
PROCEDURE
实验过程
To a pressure tube were charged tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-3-iodopyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate (563 mg, 0.8 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(1H-1,2,4-triazol-1-yl)pyridine (287 mg, 1.1 mmol), PdCl2(dppf)2.CH2Cl2 (29 mg, 0.04 mmol), DME (6 mL) and 2M Na2CO3 (2 mL). The resulting mixture was briefly degassed with Argon; the tube was capped, and heated with stirring under 80° C. overnight. After cooling, solvent was removed. The residue was diluted with EtOAc (20 ml), and organic layer was isolated, washed with brine and dried (MgSO4). After concentration under reduced pressure, the residue was purified on silica gel eluting with EtOAc/Hexanes (0-50%) to provide the title compound (370 mg, 64%).
WORKUP
后处理
- customThe resulting mixture was briefly degassed with Argon
- customthe tube was capped
- temperatureheated
- temperatureAfter cooling
- customsolvent was removed
- additionThe residue was diluted with EtOAc (20 ml)
- customorganic layer was isolated
- washwashed with brine
- dry with materialdried (MgSO4)
- concentrationAfter concentration under reduced pressure
- customthe residue was purified on silica gel eluting with EtOAc/Hexanes (0-50%)