反应详情

温度

0 °C

To a solution of 5,7-dichloro-6-(2,4,6-trifluorophenyl)-[1,2,4]triazolo[1,5-a]-pyrimidine (200 g, 0.627 mol) in anhydrous DMF (1000 mL) is added (S)-2,2,2-trifluoro-1-methyl-ethylamine (177 g, 1.57 mol). The solution is stirred from about 20° C. to about 30° C. for 24 h. The reaction mixture is added to cold water (3000 mL) slowly over 30 min. The mixture is stirred for 30 min at 10-20° C. The solid product is filtered and washed with water (2×500 mL). The crude product is dissolved into IPA (1000 mL) at 50° C. Water (2000 mL) is added to precipitate the product over 30 min. The mixture is cooled to 0° C. over 1 h and stirred for 1 h at this temperature. The solid is filtered and dried at 65° C./10 mmHg for 20 h to give a light yellow solid (204 g, 82%, 98% HPLC area purity and 99% ee).

1. stirringThe mixture is stirred for 30 min at 10-20° C
2. filtrationThe solid product is filtered
3. washwashed with water (2×500 mL)
4. dissolutionThe crude product is dissolved into IPA (1000 mL) at 50° C
5. additionWater (2000 mL) is added
6. customto precipitate the product over 30 min
7. stirringstirred for 1 h at this temperature
8. filtrationThe solid is filtered
9. customdried at 65° C./10 mmHg for 20 h
10. customto give a light yellow solid (204 g, 82%, 98% HPLC area purity and 99% ee)