Reaktion #163529

ord-cd96fb9f93694b3db7b4bb7b950145d4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigemelted in an oil bath at 120° C.
  2. 2
    workup.STIRRINGthe mixture was stirred
  3. 3
    Extraktionextracted with ethyl acetate (30 ml)
  4. 4
    Waschenwashed with saturated brine
  5. 5
    TrocknenThe extract was dried over anhydrous sodium sulfate
  6. 6
    Sonstigethe solvent was evaporated
  7. 7
    SonstigeThe obtained residue was purified by column chromatography (Yamazen HI-FLASH™ COLUMN size L, elution solvent: hexane/ethyl acetate)

Vorschrift

3,5-Dimethylpiperazine-1-carboxylic acid tert-butyl ester (1.676 g) and 2-chloropyrimidine (716 mg) were combined, melted in an oil bath at 120° C., and stirred for 5 hr 30 min. Water (10 ml) was added and the mixture was stirred, extracted with ethyl acetate (30 ml), and washed with saturated brine. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated. The obtained residue was purified by column chromatography (Yamazen HI-FLASH™ COLUMN size L, elution solvent: hexane/ethyl acetate) to give the title compound (333 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835631B2uspto-grants-2014_09