反应详情

A mixture of methyl 3,4,5-triphenyl-1H-pyrazol-1-nonanoate (3.45 g, 7.4 mmol), 5N sodium hydroxide solution (4.44 mL, 22 mmol) and methanol (60 mL) was heated at reflux for 1 hour. The solvent was evaporated, the residue diluted with water and 2N hydrochloric acid solution added until pH=1. A yellow solid was filtered off and recrystallized from dichloromethane/hexane to afford 3,4,5-triphenyl-1H-pyrazol-1-nonanoic acid hydrate (3 g, 89%); m.p.=110°-112° C. MS(CI): m/e=453 (MH+).

1. temperaturewas heated
2. temperatureat reflux for 1 hour
3. customThe solvent was evaporated
4. additionthe residue diluted with water and 2N hydrochloric acid solution
5. additionadded until pH=1
6. filtrationA yellow solid was filtered off
7. customrecrystallized from dichloromethane/hexane