反应详情

To 1-((6-methylpyridin-2-yl)methyl)-4-nitro-3-vinyl-1H-indazole (28.2 g, 95.8 mmol, Example 5, step C) in EtOH/DCM (300 mL/10 mL) was added palladium hydroxide (15 g, 20% wt). The reaction was purged with N2 and charged with hydrogen to 45 psi. The reaction was recharged during the reaction to 45 psi 4-5 times for the first 30 minutes. After 2 hours, the reaction was stopped, filtered through Celite, and the filter pad was washed with MeOH/DCM/Et3N (1 L, 10:1:1). The filtrate was concentrated and silica gel chromatography (EtOAc/hexanes 1:3) to provide the desired product (22.4 g).

1. customThe reaction was purged with N2
2. additioncharged with hydrogen to 45 psi
3. customThe reaction was recharged during the reaction to 45 psi 4-5 times for the first 30 minutes
4. filtrationfiltered through Celite
5. washthe filter pad was washed with MeOH/DCM/Et3N (1 L, 10:1:1)
6. concentrationThe filtrate was concentrated