反应详情

温度

-4 °C

In a 500 mL round bottom flask THF (50 mL) and methanol (100 mL) were taken. To the solution sodium salt of 4-oxo-4-[3-(trifluoromethyl)-5,6-dihydro[1,2,4]triazolo[4,3-a]pyrazin-7(8H)-yl]-1-(2,4,5-trifluorophenyl)butan-2-one (2.0 g) was added. It was cooled to −78 to 70° C. in a dry-ice bath. Then NaBH4 (0.7 g) was added in small lots in 10-15 min. It was stirred at −78 to 70° C. for 3-4 h. Reaction mixture was poured into aq. saturated NH4Cl solution at 0-5° C. Product was extracted with ethyl acetate. Organic layer was collected and dried over anhydrous sodium sulfate. Solvent was evaporated at reduced pressure to obtain the product. (Wt.-2.0 g, % Y-100%, % Purity by HPLC-95.6%).

1. customReaction mixture
2. extractionProduct was extracted with ethyl acetate
3. customOrganic layer was collected
4. dry with materialdried over anhydrous sodium sulfate
5. customSolvent was evaporated at reduced pressure
6. customto obtain the product