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.

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