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 stirred solution of methyl 5-acetyl-2-ethoxybenzoate (9.6 g, 0.043 mol) in a mixture of 1,4-dioxane (80 ml) and water (80 ml) was treated with 5N aqueous sodium hydroxide solution (44 ml, 0.217 mol). The mixture was stirred at room temperature for 18 hours then the solvents evaporated under vacuum. The residue was dissolved in water (100 ml), then this solution was acidified to pH 1 with concentrated hydrochloric acid and extracted with ethyl acetate (4×100 ml). The organic extracts were combined, dried (Na2SO4) and evaporated under vacuum. Crystallization of the residue from ethyl acetate gave the title compound as a colorless solid (5.4 g, 60%), m.p. 122°-125° C. Found: C,63.20; H,5.81. C11H12O4 requires C,63.45; H,5.81%.
WORKUP
后处理
- customthe solvents evaporated under vacuum
- dissolutionThe residue was dissolved in water (100 ml)
- extractionextracted with ethyl acetate (4×100 ml)
- dry with materialdried (Na2SO4)
- customevaporated under vacuum
- customCrystallization of the residue from ethyl acetate