HRID497317
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
3-{3-[4-(2,3,6-Trifluorobenzylsulfamoyl)-phenyl]-ureido}-benzimidic acid methyl ester (250 mg, 0.5 mmol) was dissolved in NH3/MeOH (15 ml, 7 M). The solution was stirred overnight at rt. Further 10 ml of NH3/MeOH (7 M) were added and the mixture stirred for 3 h at 65° C. The solvents were evaporated and the solid residue purified by flash chromatography on silica gel with a gradient of AcOEt and MeOH. The fractions with the desired product were collected, evaporated and the product crystallized from MeOH/Et2O. Yield 50%.
WORKUP
后处理
- stirringthe mixture stirred for 3 h at 65° C
- customThe solvents were evaporated
- customthe solid residue purified by flash chromatography on silica gel with a gradient of AcOEt and MeOH
- customThe fractions with the desired product were collected
- customevaporated
- customthe product crystallized from MeOH/Et2O