反应详情

温度

0 °C

A mixture of pyrazole (33.7 mg, 0.495 mmol) and sodium hydride (19.79 mg, 0.495 mmol) in N,N-dimethylformamide (DMF) (1 ml) was cooled to 0° C. and 1,1-dimethylethyl 3-bromo-5,6-dihydro[1,2,4]triazolo[4,3-a]pyrazine-7(8H)-carboxylate (50 mg, 0.165 mmol, commercially available from e.g. Allichem, Ark Pharm or Bepharm) was added. After completion of the addition, the mixture was stirred at room temp for 30 mins and then at 110° C. After 3 h, the DMF was evaporated and a few drops of NH4Cl solution were added followed by ethyl acetate (50 ml). The solution was dried (Na2SO4), filtered and concentrated. The product was purified by MDAP to give desired product in 24.1 mg.

1. additionAfter completion of the addition
2. customat 110° C
3. waitAfter 3 h
4. customthe DMF was evaporated
5. additiona few drops of NH4Cl solution were added
6. dry with materialThe solution was dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe product was purified by MDAP