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Ethyl bromopyruvate → 4-(4-Ethoxycarbonyl-thiazol-2-yl)-4-methyl-piperidine-1-carboxylic acid tert-butyl ester

HRID 871902
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 871902
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([CH3:17])([C:14](=[S:16])[NH2:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Br[CH2:19][C:20](=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22]>CCO>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([C:14]2[S:16][CH:19]=[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[N:15]=2)([CH3:17])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 66144Ethyl bromopyruvateHCID 574733781,1-Dimethylethyl 4-(aminocarbonothioyl)-4-methyl-1-piperidinecarboxylate

Produkt 1

HCID 579868564-(4-Ethoxycarbonyl-thiazol-2-yl)-4-methyl-piperidine-1-carboxylic acid tert-butyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 4-methyl-4-thiocarbamoyl-piperidine-1-carboxylic acid tert-butyl ester (1 g, 4 mmol) in EtOH (10 mL) was added ethyl bromopyruvate (0.78 g, 4 mmol) at room temperature. The mixture was heated to refluxing for 3 hours. After cooling to room temperature, the solvent was removed in vacuo. The residue was dissolved in methylene chloride (15 mL), Et3N (1 mL) and di-tert-butyl dicarbonate (1.3 g) were added to the solution. The mixture was stirred at room temperature overnight. The mixture was washed with H2O and brine. After drying (Na2SO4), the solvent was removed in vacuo, and the residue was purified by silica column chromatography with EtOAc/hexanes to afford the desired product.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto refluxing for 3 hours
  3. customthe solvent was removed in vacuo
  4. dissolutionThe residue was dissolved in methylene chloride (15 mL)
  5. additionEt3N (1 mL) and di-tert-butyl dicarbonate (1.3 g) were added to the solution
  6. washThe mixture was washed with H2O and brine
  7. dry with materialAfter drying (Na2SO4)
  8. customthe solvent was removed in vacuo
  9. customthe residue was purified by silica column chromatography with EtOAc/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-82d8202c63874ac4a105c6f2e5891940
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08975258B2

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