反应详情

温度

40 °C

To a solution of methyl 5-chloro-2-(4-(dimethylamino)benzamido)-4-(4-(3-(2-methoxyphenyl)-5-methylisoxazole-4-carbonyl)piperazin-1-yl)benzoate (108 mg, 0.171 mmol) in MeOH (1 mL) and THF (3 mL) at room temperature was added sodium borohydride (32.3 mg, 0.854 mmol). The resulting reaction mixture was stirred at 40° C. for 2 hours. The product was purified by preparative HPLC(CH3CN/H2O-10 nM ammonium acetate) to give 90 mg (81% yield) of N-(4-Chloro-2-(hydroxymethyl)-5-(4-(3-(2-methoxyphenyl)-5-methylisoxazole-4-carbonyl)piperazin-1-yl)phenyl)-4-(dimethylamino)benzamide. 1H-NMR (CDCl3, 400 MHz): δ 9.39 (1H, s), 8.03 (1H, s), 7.84 (2H, d, J=8.8 Hz), 7.58 (1H, dd, J1=7.5 Hz, J2=1.8 Hz), 7.52-7.45 (1H, m), 7.14 (1H, s), 7.11-6.99 (2H, m), 6.74 (2H, d, J=9.0 Hz), 4.71 (2H, s), 3.82 (3H, s), 3.77 (2H, s), 3.23 (2H, s), 2.97 (2H, s), 3.07 (6H, s), 2.57 (3H, s), 2.46 (2H, s).

1. customThe resulting reaction mixture
2. customThe product was purified by preparative HPLC(CH3CN/H2O-10 nM ammonium acetate)