反应详情

温度

60 °C

Combined the product of the preparation above, methyl 6-(4-(4-cyano-2-fluorophenyl)-5-methoxy-1H-pyrazol-1-yl)nicotinate (300 mg, 0.638 mmol) and lithium chloride (135 mg, 3.19 mmol) in anhydrous N-methyl-2-pyrrolidinone (5 mL) and heated at 60° C. for 16 h. Then 1.0 M aqueous lithium hydroxide (3 mL, 3.00 mmol) was added and stirred at 20° C. for 4 h. The reaction mixture was then acidified with 1 N aqueous HCl (5 mL) to form a yellow precipitate. The precipitate was collected by filtration, rinsed with water and dried under high vacuum (ca.10 Pa) to give the title compound containing 0.9 equiv. N-methyl-2-pyrrolidinone (230 mg, quantitative yield) as a brown solid. MS m/z 325 [M+H]+. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.65 (dd, J=8.2, 1.6 Hz, 1 H) 7.80 (dd, J=11.7, 1.6 Hz, 1 H) 8.24 (br. s., 1 H) 8.38-8.44 (m, 1 H) 8.52 (br. s., 2 H) 8.87-8.94 (m, 1 H) 13.40 (br. s., 1 H).

1. customto form a yellow precipitate
2. filtrationThe precipitate was collected by filtration
3. washrinsed with water
4. customdried under high vacuum (ca.10 Pa)