反应 #1253196

ord-6f410b983d4242bc8ec495f57f2e9de3

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the solution flushed with argon
  2. 2
    workup.ADDITIONPalladium (10% on carbon, 200 mg) is added
  3. 3
    过滤the mixture is filtered through celite and solvent
  4. 4
    其他removed
  5. 5
    洗涤washed twice with water
  6. 6
    干燥dried over magnesium sulfate
  7. 7
    其他the solvent is removed

实验过程

3-Fluoro-4-(4-{2-fluoroethyl}-3-oxopiperazin-1-yl)nitrobenzene (4.35 g) is dissolved in a mixture of ethyl acetate (250 ml) and DMF (5 ml), and the solution flushed with argon. Palladium (10% on carbon, 200 mg) is added and the mixture hydrogenated under ambient pressure. After gas uptake had ceased, the mixture is filtered through celite and solvent removed. The residue is taken up in ethyl acetate, washed twice with water, dried over magnesium sulfate and the solvent is removed to give 5-amino-2-[4-(2-fluoroethyl)-3-oxopiperazin-1-yl]fluorobenzene which is used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06613349B2uspto-grants-2003_09