反应详情

温度

62.5 °C

In a 50 mL three neck flask IPA (5 mL) and Dibenzoyl-L-tartaric acid monohydrate (1.84 g) were taken. It was heated to 60-65° C. 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-amine (2.0 g, % purity-90.5%) dissolved in methanol (6 mL) was added into the reaction mixture at 60-65° C. It was stirred for 30 min. at 60-65° C. Solid salt was precipitated. It was gradually cooled to room temperature over a period of 2-3 h. The salt was filtered and washed with a mixture of IPA: MeOH (2:1, 10 mL). An enantiomerically enriched desired Dibenzoyl-L-tartaric acid salt of mixture of (2R) and (2S)-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-amine was obtained (Wt.-1.72 g, % Y-45%, Purity by HPLC-99.3%, % Chiral purity by HPLC of R-isomer 81%).

1. additionwas added into the reaction mixture at 60-65° C
2. customSolid salt was precipitated
3. temperatureIt was gradually cooled to room temperature over a period of 2-3 h
4. filtrationThe salt was filtered
5. washwashed with a mixture of IPA: MeOH (2:1, 10 mL)
6. additionAn enantiomerically enriched desired Dibenzoyl-L-tartaric acid salt of mixture of (2R)