HRID967781
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 mixture of the compound (0.48 g) obtained in Step 3 of Example 1, the compound (0.44 g) obtained in Step 1, potassium carbonate (0.55 g) and anhydrous dimethylformamide (5 mL) was stirred at 95 to 105° C. for three hours under nitrogen atmosphere. Water (30 mL) was added to the resulting mixture and the residue was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate. The residue (1.1 g) obtained by removal of the solvent was purified by silica gel column chromatography (Chromatorex NH™)(eluent; hexane:ethyl acetate=1:1 to ethyl acetate) to obtain the titled compound (0.55 g) as crystals.
WORKUP
后处理
- extractionthe residue was extracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate