HRID1914728
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
30 g (0.125 mol) of ethyl (3-ethoxy-2-oxocyclohex-3-en-1-yl)(oxo)acetate were dissolved in 150 mL of glacial acetic acid and 6.5 mL of methylhydrazine (0.125 mol) were added. The mixture was stirred at room temperature for 6 hours. The solvent was then evaporated and the crude redissolved in water, made basic with 30% NH4OH and extracted with dichlormethane. The organic layer was then dried over Na2SO4 and concentrated. The residue was crystallized from diethyl ether to give 19.2 g (68% yield) of title compound.
WORKUP
后处理
- customThe solvent was then evaporated
- dissolutionthe crude redissolved in water
- extractionextracted with dichlormethane
- dry with materialThe organic layer was then dried over Na2SO4
- concentrationconcentrated
- customThe residue was crystallized from diethyl ether