1-(4-Pyridyl)piperazine → Methyl 4-[2-[4-(4-pyridyl)piperazin-1-yl]-2,2-dimethylacetyl]phenoxyacetate

HRID 743835

Reaktionsgleichung

Reaktionsgleichung von HRID 743835
[CH3:1][C:2](Br)([CH3:17])[C:3]([C:5]1[CH:16]=[CH:15][C:8]([O:9][CH2:10][C:11]([O:13][CH3:14])=[O:12])=[CH:7][CH:6]=1)=[O:4].[N:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:21][CH:20]=1>C(#N)C>[N:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:26][CH2:27][N:28]([C:2]([CH3:17])([CH3:1])[C:3]([C:5]3[CH:16]=[CH:15][C:8]([O:9][CH2:10][C:11]([O:13][CH3:14])=[O:12])=[CH:7][CH:6]=3)=[O:4])[CH2:29][CH2:30]2)=[CH:21][CH:20]=1

Komponenten

4

Edukt 2

HCID 705171-(4-Pyridyl)piperazineHCID 18918473Methyl 4-(2,2-dimethylbromoacetyl)phenoxyacetate

Produkt 1

HCID 18918600Methyl 4-[2-[4-(4-pyridyl)piperazin-1-yl]-2,2-dimethylacetyl]phenoxyacetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Methyl 4-(2,2-dimethylbromoacetyl)phenoxyacetate (1.58 g) was added to a stirred solution of 1-(4-pyridyl)piperazine (1.63 g) in acetonitrile (40 ml). After 34 days, the solid formed was removed by filtration and the filtrate evaporated to give an oil. Purification by flash chromatography on silica, eluting with 0.5 to 4.0% v/v methanol/dichloromethane gave the title compound, 240 mg, as a white foam:

Aufarbeitung

  1. customthe solid formed
  2. customwas removed by filtration
  3. customthe filtrate evaporated
  4. customto give an oil
  5. customPurification by flash chromatography on silica
  6. washeluting with 0.5 to 4.0% v/v methanol/dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-6bfdbf91bfd64b2899ae5bb585ab875f
Quelldatensatz
uspto-grants-1996_09
Patentnummer
US05556977

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