HRID2251861
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
The mixture of 2-acetyl-6-nitro-benzoic acid methyl ester (8.20 g, 36.7 mmol, Step C) and 5,5-dibromobarbituric acid (7.35 g, 25.7 mmol) in 200 mL of THF was heated to reflux under N2 for 64 h. The solvents were removed, and the residue was partitioned between EtOAc and Na2CO3(aq). The organic portion was dried over MgSO4, filtered, condensed, and the titled compound was obtained as a white solid after flash column chromatography (5 to 20% of EtOAc in hexanes).
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux under N2 for 64 h
- customThe solvents were removed
- customthe residue was partitioned between EtOAc and Na2CO3(aq)
- dry with materialThe organic portion was dried over MgSO4
- filtrationfiltered
- customcondensed