Reaktion #540154

ord-ab140c35fa8047ea8097a7d65dc39f06

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed overnight
  2. 2
    TemperaturThe reaction mixture was then cooled
  3. 3
    Einengenconcentrated under reduced pressure
  4. 4
    Sonstigethe residue was purified by column chromatography

Vorschrift

A mixture of 3-tert-butyl-1H-pyrazol-5-amine (5 g, 36 mmol, Alfa-aesar) and N,N-dimethylformamide dimethylacetal (153 mL, 1078 mmol, Aldrich) was refluxed overnight. The reaction mixture was then cooled, concentrated under reduced pressure and the residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-5% methanol in dichloromethane) to provide 6.9 g (99%) of the title compound. MS (ESI+) m/z 195 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08492371B2uspto-grants-2013_07