Cesium carbonate → 4-Bromo-1-(oxetan-3-YL)-1H-pyrazole

HRID 515904Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 515904
[Br:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.Br[CH:8]1[CH2:11][O:10][CH2:9]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH:8]2[CH2:11][O:10][CH2:9]2)[CH:6]=1

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 163754-BromopyrazoleHCID 162444933-Bromooxetane

Produkt 1

HCID 739778714-Bromo-1-(oxetan-3-YL)-1H-pyrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

4-Bromo-1H-pyrazole (1.53 g, 10.7 mmol) is dissolved in anhydrous dimethylformamide (15 mL). 3-Bromooxetane (2.0 g, 14.6 mmol) and caesium carbonate (4.7 g, 14 mmol) are successively added thereto. The reaction mixture is heated for 8 hours at 130° C. in a sealed flask. At the end of the reaction, the solvent is evaporated off in vacuo and the residue is purified by chromatography over silica gel using dichloromethane containing diethylamine and methanol as eluants to yield the expected compound.

Aufarbeitung

  1. customAt the end of the reaction
  2. customthe solvent is evaporated off in vacuo
  3. customthe residue is purified by chromatography over silica gel
  4. additioncontaining diethylamine and methanol as eluants

Quellen und Nachweise

ORD-Eintrag
ord-fc3f1cb3d3e44a0babd9c31d566c8cf5
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09108983B2

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