反应详情

A suspension of 5-chloro-7-(trifluoromethyl)[1,2,4]triazolo[1,5-a]pyridin-2-amine ((A7), 3.60 g; 15.22 mmol; 1.0 eq.), cyclopropylamine (5.27 mL; 76.1 mmol; 5.0 eq.), and N-ethyldiisopropylamine (26.22 mL; 152.2 mmol; 10.0 eq.) was heated at 80° C. in 1-butanol (36.0 mL) for 23 h., then 15 h. at 100° C. The reaction mixture was then concentrated under vacuum till dryness. Diethyl ether was added and the solid was filtered, washed with water and dried. The product was then purified by chromatography on silicagel (from 5% to 95% EtOAc in c-Hex), to give the title compound as a white solid (2.0 g; 51.1%). HPLC, Rt: 2.54 min. (purity 100%). LC/MS, M+(ESI): 258.0, M−(ESI): 256.0.

1. custom15 h.
2. customat 100° C
3. concentrationThe reaction mixture was then concentrated under vacuum till dryness
4. additionDiethyl ether was added
5. filtrationthe solid was filtered
6. washwashed with water
7. customdried
8. customThe product was then purified by chromatography on silicagel (from 5% to 95% EtOAc in c-Hex)