反应详情

Combined 1H-pyrazole-4-carbonitrile (0.432 g, 4.64 mmol) in acetone (9.28 mL), potassium carbonate (1.924 g, 13.92 mmol) and ethyl 2-bromoacetate (1.027 mL, 9.28 mmol). The reaction mixture was stirred at room temperature overnight, then concentrated in vacuo, diluted with EtOAc (10 mL), washed with water (10 mL), dried (MgSO4) and concentrated in vacuo to give a residue. The residue was purified using flash column chromatography on silica gel (EtOAc in heptane, 10-50% gradient) to give a white solid. The solid was suspended in heptane and then filtered and dried to give the title compound (0.4314 g, 51.9% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.21 (t, J=7.20 Hz, 3 H) 4.17 (q, J=7.07 Hz, 2 H) 5.19 (s, 2 H) 8.11 (s, 1 H) 8.57 (s, 1 H). MS m/z [M+H]+ 180.

1. concentrationconcentrated in vacuo
2. additiondiluted with EtOAc (10 mL)
3. washwashed with water (10 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give a residue
7. customThe residue was purified
8. customto give a white solid
9. filtrationfiltered
10. customdried