Sodium Acetate → HCID 69331771, compound

Participants

Reaction Steps

A solution of potassium cyanate (64.9 mg) in H2O (0.5 ml) was added to a solution of N′-[5-[4-(2-aminoethoxy)phenyl]-1-(4-methoxy-phenyl)-1H-pyrazol-3-yl]-N,N-dimethylurea hydrochloride (172.8 mg) and sodium acetate (65.6 mg) in a mixture of DMF (1.5 ml) and H2O (0.5 ml). The reaction mixture was stirred at ambient temperature overnight. The mixture was diluted with H2O, partitioned between AcOEt and H2O. The aqueous layer was reextracted with AcOEt. saturated aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. The residue was purified by preparative thin layer silica gel chromatography developed by 10% MeOH/CHCl3. The separated silica gel was extracted with 10% MeOH/CHCl3 and the solvent was evaporated in vacuo. The residue was crystallized from AcOEt-IPE to give N′-[5-(4-{2-[(aminocarbonyl) -amino]ethoxy}phenyl)-1-(4-methoxyphenyl)-1H-pyrazol-3-yl]-N,N-dimethylurea (87.0 mg) as a powder.

Provenance & Evidence