HRID79373

反应详情

EQUATION

反应方程式

HRID 79373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 1-((1,5-dimethyl-1H-pyrazol-3-yl)methyl)-4-nitro-3-vinyl-1H-indazole (5.15 g, 17.3 mmol) in EtOH/DCM (100 mL/10 mL) was cautiously added palladium hydroxide on carbon (2.2 g, 20% wt). The reaction mixture was purged with nitrogen and hydrogen three times each. The reaction was agitated under H2 (45 psi) for 3 hours. The system was evacuated and purged with nitrogen. The mixture was filtered through Celite and the filter pad was washed with MeOH/DCM (10:1, 300 mL). The solution was concentrated under reduced pressure and the residue was purified by silica gel chromatography (EtOAc/Hexane 2:1) to provide the product (4.35 g).

WORKUP

后处理

  1. customThe reaction mixture was purged with nitrogen and hydrogen three times each
  2. customThe system was evacuated
  3. custompurged with nitrogen
  4. filtrationThe mixture was filtered through Celite
  5. washthe filter pad was washed with MeOH/DCM (10:1, 300 mL)
  6. concentrationThe solution was concentrated under reduced pressure
  7. customthe residue was purified by silica gel chromatography (EtOAc/Hexane 2:1)