反应详情

温度

130 °C

A mixture of methyl 4-fluorobenzoate (2 g, 0.0130 mol), pyrazole (1.33 g, 0.0195 mmol) and potassium carbonate (3.59 g, 0.0260 mol) in dry 1-methyl-1-pyrrolidinone (20 mL) was heated to 130° C. for 44 hours. The cooled reaction mixture was then partitioned between ethyl acetate (200 mL) and 2 M sodium hydroxide (200 mL). The organic phase was separated, washed with 2 M sodium hydroxide (200 mL), 2 M hydrochloric acid (2×200 mL), water (200 mL), and brine (200 mL), dried over anhydrous magnesium sulfate, and concentrated in vacuo to afford a white solid (0.71 g). Recrystallization from hexane (40 mL) gave the title compound (0.533 g, 20%) as a white crystalline solid, m.p. 115° C.

1. customThe cooled reaction mixture
2. customwas then partitioned between ethyl acetate (200 mL) and 2 M sodium hydroxide (200 mL)
3. customThe organic phase was separated
4. washwashed with 2 M sodium hydroxide (200 mL), 2 M hydrochloric acid (2×200 mL), water (200 mL), and brine (200 mL)
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo