反应详情

温度

100 °C

Methyl 5-methyl-2-(1-methyl-1H-pyrazol-4-yl)benzoate (˜1 g, ˜4.41 mmol) was dissolved in MeOH/H2O (4:1, 50 mL) and then LiOH (0.36 g, 15 mmol) was added. The mixture was heated at reflux for 2 h at 100° C. The analytical HPLC indicated the starting material was consumed, the mixture was cooled to 0° C. and 2 M HCl solution was added bring the pH ˜4. MeOH was removed in vacuo and the acid was precipitated. The acid was collected by filtration and dried in vacuo and used without further purification. ESI-MS (m/z): 217 [M+1]+. 1H NMR (300 MHz, DMSO-d6) δ 12.87 (br s, 1H), 7.82 (s, 1H), 7.51 (s, 1H), 7.39-7.27 (m, 3H), 3.85 (s, 3H), 2.32 (s, 3H).

1. temperatureThe mixture was heated
2. customwas consumed
3. temperaturethe mixture was cooled to 0° C.
4. addition2 M HCl solution was added
5. customMeOH was removed in vacuo
6. customthe acid was precipitated
7. filtrationThe acid was collected by filtration
8. customdried in vacuo
9. customused without further purification