反応 #8170

ord-96385c6264c1424398d9348e12f7a5f7

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed under vacuum
  2. 2
    洗浄washed with water (twice) and saturated sodium bicarbonate (once), and the organic layer
  3. 3
    乾燥dried over magnesium sulfate (MgSO4)
  4. 4
    ろ過The solid was filtered
  5. 5
    その他the solvents removed under vacuum
  6. 6
    その他The reaction product was purified over silica gel

実験手順

To 1-(4-nitrophenyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (0.5 g, 1.5 mmol) dissolved in methanol (4 mL) was added palladium on carbon and ammonium formate (0.428 g, 6.8 mmol). This mixture was stirred at room temperature overnight. The solvent was removed under vacuum, then the material was resuspended in chloroform, and washed with water (twice) and saturated sodium bicarbonate (once), and the organic layer dried over magnesium sulfate (MgSO4). The solid was filtered and the solvents removed under vacuum. The reaction product was purified over silica gel to yield the named product (m.p. 102° C.–103° C.).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087634B2uspto-grants-2006_08