反应详情

温度

125 °C

A mixture of the product from example 13, step 2 (0.73 g, 3.68 mmol), benzyl alcohol (9.4 g, 87 mmol) and K-t-BuO was stirred at 125° C. for 4.5 h. The reaction mixture was purified by silica gel chromatography (13×5 cm) using CHCl3/MeOH (7:3 followed by 9:1) as eluent. Solvents were evaporated off and the residue was redissolved in ethyl acetate. Filtration and concentration in vacuo furnished 0.90 g (90%) of the title compound as a beige oil. HRMS m/z calcd for C15H18N4O (M)+ 270.1481, found 270.1482. Anal. (C15H18N4O) C, H, N. *This compound was also characterized as its maleate salt: mp 155-156° C. HRMS m/z calcd for C15H18N4O (M)+ 270.1481, found 270.1482. Anal. (C15H18N4O.C4H4O4) C, H, N.

1. customThe reaction mixture was purified by silica gel chromatography (13×5 cm)
2. customSolvents were evaporated off
3. dissolutionthe residue was redissolved in ethyl acetate
4. filtrationFiltration and concentration in vacuo