Reaktion #435025

ord-d624d13d299b414d882b057397a26ea0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGat the same temperature, and the reaction mixture was stirred for 1 hour at 60° C
  2. 2
    SonstigeAfter completion of the reaction
  3. 3
    workup.ADDITIONthe reaction mixture was gradually added to ice, extraction
  4. 4
    Extraktionthe organic extract
  5. 5
    Waschenwas washed with water and brine
  6. 6
    Trocknendried over anhydrous magnesium sulfate
  7. 7
    Filtrationfiltered
  8. 8
    Sonstigethe solvent was evaporated under reduced pressure

Vorschrift

Sodium hydride (60% in oil; 24.6 mg) was added to a solution of tert-butyl N-(7-bromo-2-methoxypyrazolo[1,5-a]pyridin-3-yl)carbamate (140 mg) in N,N-dimethylformamide (10 mL) at room temperature and the reaction mixture was stirred for 30 minutes. (Bromomethyl)cyclopropane (0.06 mL) was added thereto at the same temperature, and the reaction mixture was stirred for 1 hour at 60° C. After completion of the reaction, the reaction mixture was gradually added to ice, extraction was performed with ethyl acetate, the organic extract was washed with water and brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure to afford a crude product of tert-butyl N-(7-bromo-2-methoxypyrazolo[1,5-a]pyridin-3-yl)-N-cyclopropylmethylcarbamate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07176216B2uspto-grants-2007_02