HRID1524873
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
- 90 °C
PROCEDURE
实验过程
The product from Example 143 Part A (1.0 g, 4.0 mmol), Zn(CN)2 (0.52 g, 4.8 mmol), Pd(PPh3)4 (0.23 g, 0.2 mmol) were added together with 9 mL of DMF. The mixture was degassed and then heated at 90° C. for 6 h. Water and EtOAc were added to the reaction mixture. It was filtered to remove inorganic solids. The layers were separated and the EtOAc layer was washed with water and brine. It was dried over MgSO4, concentrated, and purified by flash chromatography (silica, EtOAc/hexane) to give 0.28 g of the desired product. MS: 196.1 (M+1)+.
WORKUP
后处理
- customThe mixture was degassed
- additionWater and EtOAc were added to the reaction mixture
- filtrationIt was filtered
- customto remove inorganic solids
- customThe layers were separated
- washthe EtOAc layer was washed with water and brine
- dry with materialIt was dried over MgSO4
- concentrationconcentrated
- custompurified by flash chromatography (silica, EtOAc/hexane)