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Potassium Carbonate → 4-[Ethoxycarbonyl-(3-trifluoromethyl-phenyl)-methyl]-piperazine-1-carboxylic acid tert-butyl ester

HRID 550841
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 550841
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:14](=O)([O-])[O-].[K+].[K+].[CH3:20][O:21][C:22](=[O:35])[CH:23](Br)[C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([C:30]([F:33])([F:32])[F:31])[CH:25]=1>CN(C)C=O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH:23]([C:22]([O:21][CH2:20][CH3:14])=[O:35])[C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([C:30]([F:33])([F:32])[F:31])[CH:25]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 19796654Methyl 2-bromo-2-[3-(trifluoromethyl)phenyl]acetate

Produkt 1

HCID 671519624-[Ethoxycarbonyl-(3-trifluoromethyl-phenyl)-methyl]-piperazine-1-carboxylic acid tert-butyl esterAusbeute 74,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel

Versuchsvorschrift

A mixture of Piperazine-1-carboxylic acid tert-butyl ester (1.80 g, 9.68 mmol), potassium carbonate (2.0 g, 14.5 mmole) and Bromo-(3-trifluoromethyl-phenyl)-acetic acid methyl ester (3.0 g, 9.65 mmol) in N,N-dimethylformamide (40 mL) was stirred at room temperature overnight. Concentration gave a crude material which was partitioned between methylene chloride and water. The organic layer was dried over magnesium sulfate and concentrated to give an oil. The crude oil was loaded onto an Isco 120 g column and eluted using 20% ethyl acetate/hexanes to yield 4-[Ethoxycarbonyl-(3-trifluoromethyl-phenyl)-methyl]-piperazine-1-carboxylic acid tert-butyl ester (3.0 g, 74% yield) as a colorless oil. The NMR spectrum obtained on the sample is compatible with its structure.

Aufarbeitung

  1. concentrationConcentration
  2. customgave a crude material which
  3. customwas partitioned between methylene chloride and water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customto give an oil
  7. washeluted

Quellen und Nachweise

ORD-Eintrag
ord-6da0332748724a9e8cbd7cf430ac0c51
Quelldatensatz
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07947692B2

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