These common heterocyclic compound, 1572-10-7, name is 3-Amino-5-phenylpyrazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Quality Control of 3-Amino-5-phenylpyrazole
To a cold (0C) solution of 3-amino-5-phenylpyrazole (10.0 g, 62.8 mmol) in toluene (100 mL) was added ethoxycarbonyl isothiocyanate (8.3 mL, 70 mmol) dropwise via a pressure equalizing funnel. Upon complete addition, the cold bath was removed and the resulting solution was stirred at room temperature for 15 hours, at which time a heavy white precipitate had formed. The precipitate was collected by filtration and dried to give ethyl [ (3-phenyl-1 H-pyrazol-5-yl) amino] carbothioylcarbamate (11 g, 60%) as a white solid.’H-NMR (DMSO-d6) : 8 13.25 (s, 1H), 12.06 (s, 1 H), 11.40 (s, 1H), 7.75 (d, 2H), 7.5-7. 3 (m, 4H), 4.25 (q, 2H), 1.29 (t, 3H); MS m/z 291 (M+1).
The synthetic route of 3-Amino-5-phenylpyrazole has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2003/76441; (2003); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics