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
In a test tube for wicrowave reactor, a solution of 0.20 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methyl benzoic acid amide synthesized in Step 1 of Synthetic Example 19, 0.10 g of 5-bromopyrimidine, 4.8 mg of copper iodide, 0.21 g of potassium phosphate and 4.4 mg of N,N-dimethyl ethylene diamine in 1 mL of 1,4-dioxane was placed, and reacted by use of a microwave focused chemical synthesizer (Discover manufactured by CEM Corporation) at 120 W and 120° C. for 20 minutes. After the completion of the reaction, insoluble material was removed through silica gel column, and the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:1) to obtain 0.13 g of the aimed product as white crystal.
WORKUP
后处理
- customreacted by use of a microwave
- customat 120 W and 120° C.
- customfor 20 minutes
- customAfter the completion of the reaction, insoluble material
- customwas removed through silica gel column
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified with silica gel column chromatography that