反应详情

To a slurry of tert-butyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate (3.6 g, 8.89 mmol) and 1-(4-chlorophenyl)cyclopropanamine (1.491 g, 8.89 mmol) in THF (50 mL) was stirred for 5 h at 80° C. The precipitate was filtrated through a plug washing with THF to give acrude product that was purified by Biotage eluting with 4/1-hexane/ethyl acetate to give 1.8 g of tert-butyl 4-(4-(1-(4-chlorophenyl)cyclopropylamino)-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate as a solid. LC-MS (Condition A), MS m/z (M++H) 536.0. A solution of above tert-butyl 4-(4-(1-(4-chlorophenyl)cyclopropylamino)-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate (4 g, 7.46 mmol) and HCl in dioxane (7.46 ml, 4 M) was stirred for 4 h. Concentration gav 3.58 g of the desired product as a solid, LC-MS (Condition A), MS m/z (M++H) 480.05.

1. filtrationThe precipitate was filtrated through a plug
2. washwashing with THF
3. customto give acrude product that
4. customwas purified by Biotage
5. washeluting with 4/1-hexane/ethyl acetate