HRID1661786
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
Diethyl malonate (400 μL) was added to a mixture of 6-iodo-[1,2,4]triazolo[1,5-α]pyridine (245 mg, 1 mmol), copper iodide (19 mg, 0.1 mmol), biphenyl-2-ol (34 mg, 0.2 mmol), and Cs2CO3 in THF (5 mL). The hetereogeneous solution was stirred for 16 h at 70° C. After cooling, the mixture was partitioned between chloroform (40 mL) and aq NH4Cl (20 mL). The organic layer was washed with NH4Cl (3×15 mL), NaHCO3 (20 mL), and brine (20 mL) then was dried over Na2SO4. Concentration of the solution followed by SiO2 flash chromatography purification yielded the product (170 mg, 61%) as a colorless glass.
WORKUP
后处理
- temperatureAfter cooling
- customthe mixture was partitioned between chloroform (40 mL) and aq NH4Cl (20 mL)
- washThe organic layer was washed with NH4Cl (3×15 mL), NaHCO3 (20 mL), and brine (20 mL)
- dry with materialthen was dried over Na2SO4
- customConcentration of the solution followed by SiO2 flash chromatography purification