反应详情

温度

100 °C

To a reaction vial was added 1-benzyl-3-bromo-4-nitro-1H-indazole (100 mg, 0.301 mmol), cyclopropylboronic acid (33.6 mg, 0.391 mmol) and potassium phosphate (192 mg, 0.903 mmol). Toluene (1.5 mL) and water (0.1 mL) were added. The mixture was purged with argon for 30 minutes. Palladium (II) acetate (3.38 mg, 0.0151 mmol) and tri-cyclohexyl phosphine (8.44 mg, 0.0301 mmol) were added. The reaction vessel was purged with argon and sealed. The mixture was heated at 100° C. for 24 hours. The mixture was filtered through glass fiber filter paper, washing with ethyl acetate and methanol followed by concentration under reduced pressure. The material was purified by preparative chromatography on silica, eluting with hexane/ethyl acetate (5:1). The band containing the desired product was isolated and concentrated under reduced pressure to give 1-benzyl-3-cyclopropyl-4-nitro-1H-indazole (60.5 mg).

1. customThe mixture was purged with argon for 30 minutes
2. customThe reaction vessel was purged with argon
3. customsealed
4. filtrationThe mixture was filtered through glass fiber
5. filtrationfilter paper
6. washwashing with ethyl acetate and methanol
7. concentrationfollowed by concentration under reduced pressure
8. customThe material was purified by preparative chromatography on silica
9. washeluting with hexane/ethyl acetate (5:1)
10. additionThe band containing the desired product
11. customwas isolated
12. concentrationconcentrated under reduced pressure