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
A solution of 6 g of 2,4-Dichloro-1-iodo-benzene, 15.7 g of Cs2CO3, 63 mg of Pd(dba)2 (Bis(dibenzylidenacetonpalladium), 127 mg of Xantphos (9,9-Dimethyl-4,5-bis(diphenylphosphino)xanthene) and 8.3 g of 1-(4-Trifluoromethyl-phenyl)ethanone in 45 ml of dioxane was heated under argon for 30 min at 150° C. by microwave irradiation. After cooling to room temperature and dilution with saturated aqueous sodium hydrogen carbonate solution, the reaction mixture was filtered through a chem Elut® cartridge by eluting with ethyl acetate. The solvents were removed under reduced pressure and the crude product was purified by chromatography on silica gel eluting with a gradient of n-heptane/ethyl acetate. The fractions containing the product were combined and the solvent evaporated under reduced pressure. Yield: 9.1 g.
WORKUP
后处理
- filtrationdilution with saturated aqueous sodium hydrogen carbonate solution, the reaction mixture was filtered through a chem Elut® cartridge
- washby eluting with ethyl acetate
- customThe solvents were removed under reduced pressure
- customthe crude product was purified by chromatography on silica gel eluting with a gradient of n-heptane/ethyl acetate
- additionThe fractions containing the product
- customthe solvent evaporated under reduced pressure