HRID2280856
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
- 115 °C
PROCEDURE
实验过程
To a solution of compound 2b (3.1 g, 5 mmol) in DMF (50 mL) were added under argon atmosphere Zn(CN)2 (500 mg, 4.3 mmol), Pd2(dba)3 (300 mg, 0.33 mmol) and Xantphos (150 mg, 0.31 mmol). The mixture was stirred for 10 h at 115° C. under microwave irradiation. After cooling to rt the reaction mixture was diluted with water (250 mL) and extracted with EA (250 mL×2). The combined organic layers were washed with brine (100 mL×3) and dried over Na2SO4. The residue was purified by CC (EA/PE) to give the title compound 2c (1.2 g, 42%) as a pale yellow solid.
WORKUP
后处理
- temperatureAfter cooling to rt the reaction mixture
- extractionextracted with EA (250 mL×2)
- washThe combined organic layers were washed with brine (100 mL×3)
- dry with materialdried over Na2SO4
- customThe residue was purified by CC (EA/PE)