反应详情

温度

170 °C

1H-NMR(400 MHz, CDCl3) δ: 3.87(3H, s), 4.78(2H, d, J=5.0 Hz), 5.75(1H, t, J=5.0 Hz), 6.87(1H, d, J=8.5 Hz), 7.31(1H, dd, J=8.5, 2.0 Hz), 7.43(1H, d, J=2.0 Hz), 8.05(1H, dd, J=8.5, 1.5 Hz), 8.24(1H, dd, J=1.5, 1.0 Hz), 8.29(1H, dd, J=8.5, 0.5 Hz). 10.0 g of 1-chloro-4-(3-chloro-4-methoxybenzyl)amino-6-cyanophthalazine was dissolved in 50 ml of N-methyl-2-piperidone. After adding 43.32 g of 4-hydroxypiperidine and 10 ml of diisopropylethylamine, the resulting mixture was heated at 170° C. for 8 hours. Then ethyl acetate wag added thereto and the resulting mixture was successively washed for three times with water and once with brine and dried over anhydrous magnesium sulfate. After evaporating the solvent, the residue was purified by silica gel column chromatography (methylene chloride:methanol=30:1) to give 10.1 g of 4-(3-chloro-4-methoxybenzyl)amino-6-cyano-1-(4-hydroxypiperidino)phthalazine as yellow crystals. M.p.: 172.0-173.5° C., Mass 424(MH+),

1. washthe resulting mixture was successively washed for three times with water and once with brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customAfter evaporating the solvent
4. customthe residue was purified by silica gel column chromatography (methylene chloride:methanol=30:1)