反应详情

温度

62.5 °C

In a 100 mL three neck flask IPA (25 mL) and Dibenzoyl-D-tartaric acid (8.8 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 (10 g, purity-91.8%) dissolved in methanol (30 mL) was added slowly into the reaction mixture at 60-65° C. It was stirred for 1 h at 60-65° C. Solid salt was precipitated. It was gradually cooled to room temperature and stirred for 3 h. The salt was filtered and washed with a mixture of IPA: MeOH (2:1). An enantiomerically enriched desired Dibenzoyl-D-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.-7.2 g, % Y-38.4%, Purity by HPLC-98.2%, % Chiral purity by HPLC of S-isomer 71.7%).

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