HRID1700285
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
A mixture of 3-bromo-6-((4-methoxybenzyl)oxy)benzaldehyde (4 g), Zn(CN)2 (1 g) and Pd(PPh3)4 (4.32 g) in 40 mL DMF was stirred at 90° C. for 3 hours, cooled to ambient temperature and diluted with 100 mL 50% NH4OH. The aqueous layer was extracted with ethyl acetate (3×). The organic layer was dried, concentrated and purified on silica gel column (ethyl acetate/hexane, 1:4) to afford 2.8 g of 3-cyano-6-((4-methoxybenzyl)oxy)benzaldehyde as a yellow solid.
WORKUP
后处理
- temperaturecooled to ambient temperature
- extractionThe aqueous layer was extracted with ethyl acetate (3×)
- customThe organic layer was dried
- concentrationconcentrated
- custompurified on silica gel column (ethyl acetate/hexane, 1:4)