6-Nitroindazole → 3-bromo-6-nitro-1H-indazole

To a solution of 5.0 g of 6-nitro-1H-indazole in 50 ml dimethylformamide was added 5.73 g of N-bromosuccinimide at room temperature, and the mixture was stirred at the same temperature for 1 hour. After removing the solvent by distillation, the residue was added with 250 ml of ethyl acetate. The mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine, and dried over anhydrous magnesium sulfate. After filtrating the organic layer through a silica gel pat, the solvent was evaporated and the resulting crystals were suspended in toluene, to give 6.59 g of the title compound as light brown crystals.

1. customAfter removing the solvent
2. distillationby distillation
3. additionthe residue was added with 250 ml of ethyl acetate
4. washThe mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationAfter filtrating the organic layer through a silica gel pat
7. customthe solvent was evaporated

ORDレコード

ord-268b83e76465476298afe249a5d4db9d

出典データセット

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07776890B2