Reaktion #2180253

ord-2b6a36a2e8c0433680e5e0eb97cf45a2

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeReaction mixture
  2. 2
    Sonstigewas brought to room temperature
  3. 3
    SonstigeReaction mixture
  4. 4
    Einengenwas concentrated
  5. 5
    workup.ADDITIONdiluted with water
  6. 6
    Extraktionextracted dichloromethane
  7. 7
    Waschenwashed with brine solution
  8. 8
    Trocknendried over anhydrous Na2SO4
  9. 9
    EinengenConcentrated
  10. 10
    Sonstigepurified by column chromatography

Vorschrift

Triethyl amine (1.0 eq) was added to solution of N-(2-aminophenyl)-4,5,6,7-tetrahydro[1,3]thiazolo[5,4-c]pyridine-2-carboxamide obtained in step VIII of example I (1.0 mmol) in 10 mL THF. The solution was cooled to 0° C. 4-Methyl-benzenesulfonyl chloride (1.0 mmol) was added slowly with continuous stirring. Reaction mixture was brought to room temperature and stirred for 2 h Reaction mixture was concentrated, diluted with water, extracted dichloromethane, washed with brine solution, and dried over anhydrous Na2SO4. Concentrated and purified by column chromatography to yield the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08440830B2uspto-grants-2013_05