HRID857320
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
To a solution of 1.4 g of the acid of Step 5 in quinoline (10 mL) was added 100 mg of copper powder. The reaction mixture was heated to reflux and stirred for 2 hours. The copper powder was removed by filtration and 6N HCl was added to the filtrate. The aqueous layer was extracted with EtOAc and the combined organic layers were dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography eluted with 10% EtOAc in Hexanes to provide 750 mg of the title compound as an orange solid foam.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux
- customThe copper powder was removed by filtration and 6N HCl
- additionwas added to the filtrate
- extractionThe aqueous layer was extracted with EtOAc
- dry with materialthe combined organic layers were dried over Na2SO4
- concentrationconcentrated
- customThe residue was purified by silica gel chromatography
- washeluted with 10% EtOAc in Hexanes