反応 #1253196

ord-6f410b983d4242bc8ec495f57f2e9de3

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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