HRID485680

反应详情

EQUATION

反应方程式

HRID 485680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat vigorous reflux for three hours
  2. temperatureto cool
  3. extractionwhereupon ethyl acetate extraction
  4. customby drying
  5. custom(MgSO4) and evaporation