反应详情

温度

50 °C

A mixture of ethyl 1H-pyrazole-4-carboxylate (400 mg, 2.85 mmol), K2CO3 (1.97 g, 14.3 mmol) and 4-methoxybenzyl bromide (0.453 ml, 3.14 mmol) in dry acetone (10 ml) was heated to 50° C. for 3 h. The reaction mixture was filtered, and the filtrate was concentrated. EtOH (10 mL) and KOH (320 mg, 5.71 mmol) were added and the mixture was heated to 65° C. for 6 h, before it was concentrated again. The crude product was dissolved in water (5 ml), washed with EA (2×10 ml) and acidified with 1N HCl. The resulting precipitate was collected by filtration, washed with water and dried in vacuo affording the title compound. LCMS RtL=0.86 min, [M+H]+=233.2.

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate was concentrated
3. temperaturethe mixture was heated to 65° C. for 6 h, before it
4. concentrationwas concentrated again
5. dissolutionThe crude product was dissolved in water (5 ml)
6. washwashed with EA (2×10 ml)
7. filtrationThe resulting precipitate was collected by filtration
8. washwashed with water
9. customdried in vacuo