HRID25394

反应详情

EQUATION

反应方程式

HRID 25394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureto reflux for two hours
  2. customis then brought back to a temperature in the region of 25° C.
  3. filtrationfiltered through Celite® through a sintered glass funnel
  4. customThe solid obtained
  5. washis washed with methanol
  6. concentrationthe filtrate is concentrated by evaporation under reduced pressure
  7. customThe oil thus obtained
  8. washThe organic phase is washed with two times 60 ml of distilled water
  9. customthe aqueous phases thus obtained
  10. extractionare extracted with 80 ml of dichloromethane
  11. dry with materialThe pooled organic phases are dried over magnesium sulfate
  12. filtrationfiltered
  13. concentrationconcentrated by evaporation under reduced pressure