反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5-Amino-N-cyclohexyl-1H-indazole-3-carboxamide can be obtained in the following way: a suspension of 1.57 g of N-cyclohexyl-5-nitro-1H-indazole-3-carboxamide, of 80 ml of methanol, of 1.37 g of ammonium formate and of 0.314 g of palladium hydroxide is brought to reflux for two hours. The reaction medium is then brought back to a temperature in the region of 25° C. and filtered through Celite® through a sintered glass funnel. The solid obtained is washed with methanol and the filtrate is concentrated by evaporation under reduced pressure. The oil thus obtained is taken up with 80 ml of dichloromethane and 80 ml of water. The organic phase is washed with two times 60 ml of distilled water and the aqueous phases thus obtained are extracted with 80 ml of dichloromethane. The pooled organic phases are dried over magnesium sulfate, filtered and concentrated by evaporation under reduced pressure. 1.17 g of 5-amino-N-cyclohexyl-1H-indazole-3-carboxamide are thus obtained in the form of a pale pink solid (Rf=0.40, silica gel thin layer chromatography, eluent: dichloromethane/methanol (9/1 by volume)).
WORKUP
后处理
- temperatureto reflux for two hours
- customis then brought back to a temperature in the region of 25° C.
- filtrationfiltered through Celite® through a sintered glass funnel
- customThe solid obtained
- washis washed with methanol
- concentrationthe filtrate is concentrated by evaporation under reduced pressure
- customThe oil thus obtained
- washThe organic phase is washed with two times 60 ml of distilled water
- customthe aqueous phases thus obtained
- extractionare extracted with 80 ml of dichloromethane
- dry with materialThe pooled organic phases are dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated by evaporation under reduced pressure