反应详情

温度

60 °C

Ethyl 1H,2′H-3,3′-bipyrazole-5-carboxylate (1.959 mmol, 0.404 g) was dissolved in ethanol (5 ml) and cooled in an ice bath. NaOH 1 M solution (1.959 mmol, 4 ml) was slowly added. The solution was heated to 60° C. for 1 h. Ethanol was removed under vacuum and the residue was diluted with tert-butyl methyl ether. The solution was again cooled with an ice bath and acidified with 2 N HCl solution. The solution was allowed to warm to ambient temperature and stirred overnight. Water and DCM was added and the phases were separated. Both phases were evaporated and combined. 0.551 g of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 6.70 (d, 1H), 7.04 (s, 1H), 7.77 (d, 1H).

1. temperaturecooled in an ice bath
2. customEthanol was removed under vacuum
3. additionthe residue was diluted with tert-butyl methyl ether
4. temperatureThe solution was again cooled with an ice bath
5. temperatureto warm to ambient temperature
6. additionWater and DCM was added
7. customthe phases were separated
8. customBoth phases were evaporated