HRID497317

反应详情

EQUATION

反应方程式

HRID 497317 的结构方程式

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

  1. stirringthe mixture stirred for 3 h at 65° C
  2. customThe solvents were evaporated
  3. customthe solid residue purified by flash chromatography on silica gel with a gradient of AcOEt and MeOH
  4. customThe fractions with the desired product were collected
  5. customevaporated
  6. customthe product crystallized from MeOH/Et2O