反应详情

To a solution of ammonium thiocyanate (17.8 g, 0.234 mol) in dry acetone (200 ml) at 0° C. under nitrogen is added benzoylchloride (30 g, 0.213 mol) over a period of 15 min. The reaction mixture is stirred at rt for 30 min and filtered. To the filtrate is added 3-aminopyrazole (14.1 g, 0.17 mol) dropwise and stirred 3 h at room temperature. The solvents are removed under vacuum and the residue is purified by flash chromatography using chloroform/methanol (9/1) as eluent. N-[(1H-pyrazol-3-ylamino)carbonothioyl]benzamide is isolated as a solid (22 g; 52%). M+ (ESI): 246.9. TLC—Chloroform/methanol (9/1): Rf−0.45.

1. filtrationfiltered
2. stirringstirred 3 h at room temperature
3. customThe solvents are removed under vacuum
4. customthe residue is purified by flash chromatography