HRID49131
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
PROCEDURE
实验过程
Tetrakis(triphenylphosphine)palladium (1 g) was added to a mixture of 5 g of 4-methoxyphenylboronic acid, 6.6 g of 5-bromo-2-fluoronitrobenzene and 30 mL of 2M sodium carbonate solution in 50 mL of toluene and 50 mL of ethanol. The mixture was heated to reflux for 2 hours, concentrated, and the residue extracted twice with ethyl acetate. The ethyl acetate layer was washed with water, brine, dried, and concentrated to give a brown oily solid. The solid was purified by column chromatography on silica gel in 5% ethyl acetate in hexane to give crude-4-fluoro-4′-methoxy-3-nitrobiphenyl as a pale yellow solid.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 2 hours
- concentrationconcentrated
- extractionthe residue extracted twice with ethyl acetate
- washThe ethyl acetate layer was washed with water, brine
- customdried
- concentrationconcentrated
- customto give a brown oily solid
- customThe solid was purified by column chromatography on silica gel in 5% ethyl acetate in hexane