반응 #8170

ord-96385c6264c1424398d9348e12f7a5f7

반응 방정식

O=C[O-].[NH4+]
ammonium formate
CCOC(=O)c1cnn(-c2ccc([N+](=O)[O-])cc2)c1C(F)(F)F
1-(4-nitrophenyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester
CCOC(=O)c1cnn(-c2ccc(N)cc2)c1C(F)(F)F
product
CCOC(=O)c1cnn(-c2ccc(N)cc2)c1C(F)(F)F
1-(4-aminophenyl)-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was removed under vacuum
  2. 2
    세척washed with water (twice) and saturated sodium bicarbonate (once), and the organic layer
  3. 3
    건조dried over magnesium sulfate (MgSO4)
  4. 4
    여과The solid was filtered
  5. 5
    기타the solvents removed under vacuum
  6. 6
    기타The reaction product was purified over silica gel

실험 절차

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087634B2uspto-grants-2006_08