(Methoxycarbonylsulfamoyl)triethylammonium hydroxide → US9290457, Example 6

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Reaction Steps

2-[5-Acetyl-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidin-4-yl]-5-cyano-benzoic acid formyl hydrazide (intermediate 11) (30.0 mg, 0.06 mmol)) is suspended in dichloromethane (1 mL) and (methoxycarbonylsulfamoyl)triethyl-ammonium hydroxide (Burgess reagent)(35.8 mg, 0.15 mmol) is added. The mixture is stirred at room temperature for 3 days. Additional (methoxycarbonylsulfamoyl)triethyl-ammonium hydroxide (Burgess reagent)(35.8 mg, 0.15 mmol) is added and the reaction is continued for 2 h at 40° C. The solvent is removed under reduced pressure and purification is performed by reversed phase HPLC. Yield: 4 mg; ESI mass spectrum [M+H]+=482; Retention time HPLC: 1.02 min (HPLC method Z018_S04).

Provenance & Evidence