HRID485680
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
4-Ethoxycarbonyl-1-phenyl-3-pyrazolin-5-one (2.139 g, 9.2 mmol) in 1N sodium hydroxide (50 ml) was stirred under nitrogen at vigorous reflux for three hours. The reaction mixture was allowed to cool and acidified (HCl) to pH 3.5, whereupon ethyl acetate extraction, followed by drying (MgSO4) and evaporation produced the desired product (1.072 g, 72%) δ max(CHCl3) 1705, 1595, 1495 cm-1 δ(D6 -DMSO) 5.60 (1H,d,J2 Hz, C4 proton), 7.60 (6H, m, phenyl protons and C3 proton) Found; M+ ; 160.0641. C9H8N2O6 requires M; 160.0637.
WORKUP
后处理
- temperatureat vigorous reflux for three hours
- temperatureto cool
- extractionwhereupon ethyl acetate extraction
- customby drying
- custom(MgSO4) and evaporation