反应详情

To a solution of 3-amino-1H-pyrazole-4-carbonitrile (1.211 g, 11.21 mmol) in anhydrous DMF (20 ml) K2CO3 (5.414 g, 39.24 mmol) was added. The suspension was stirred 5 min at room temperature and treated with p-bromomethylbenzoic acid methyl ester (2.568 g, 11.21 mmol), stirred for 2.5 hrs at 100° C., cooled and filtered. Filtrate was evaporated to form an oily residue, which was dissolved in a mixture Et2O-acetone and kept overnight at −10° C. A crystalline material was formed which was triturated with hot EtOAc, again kept overnight at −10° C. and was collected by filtration to form the title compound 95 (675 mg, 24% yield). LRMS: 256.3 (calc.), 257.3 (found).

1. stirringstirred for 2.5 hrs at 100° C.
2. temperaturecooled
3. filtrationfiltered
4. customFiltrate was evaporated
5. customto form an oily residue, which
6. waitkept overnight at −10° C
7. customA crystalline material was formed which
8. customwas triturated with hot EtOAc, again kept overnight at −10° C.
9. filtrationwas collected by filtration