反应详情

温度

130 °C

2-Chloro-N-[3-(2-pyrrolidin-1-yl-ethoxy)-4-trifluoromethyl-phenyl]-nicotinamide (199.1 mg), DIEA (252 μL) and 4-fluorobenzylamine (193 μL) were combined in a sealed tube and heated to 130° C. for 2 h. The mixture was purified on silica gel chromatography (2-3.5% MeOH/CH2Cl2). The desired fractions were concentrated in vacuo, and the residue was dissolved in Et2O and hexanes were added until the solution became cloudy. The solids were filtered, and dried. Additional material was obtained from the filtrate upon additional rounds of concentration, dissolving in Et2O and treatment with hexanes. M+H 503.4, Calc'd for C26H26N4O2F4-502.2.

1. customThe mixture was purified on silica gel chromatography (2-3.5% MeOH/CH2Cl2)
2. concentrationThe desired fractions were concentrated in vacuo
3. dissolutionthe residue was dissolved in Et2O
4. additionhexanes were added until the solution
5. filtrationThe solids were filtered
6. customdried
7. customAdditional material was obtained from the filtrate upon additional rounds of concentration