Réaction #1099225

ord-fa4d49b87a9c492fa7a9777c3bc618ad

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températureunder reflux for 6 hours
  2. 2
    workup.STIRRINGstirring
  3. 3
    AutreThe formed piperidine hydrochloric salt was separated by filtration
  4. 4
    Autrethe solvent removed with a rotary evaporator
  5. 5
    workup.ADDITIONThe resulting precipitate containing the crude product
  6. 6
    Autrewas recrystallized with toluene
  7. 7
    Autreto obtain a dark powder

Mode opératoire

0.5 g (1.07 mmol) 2-{[4-chloro-2-((E)-{4-[ethyl(2-hydroxyethyl)amino]phenyl}-diazenyl)-1,3-thiazol-5-yl]methylene}-1H-indene-1,3(2H)-dione were dissolved in 20 ml THF. Then 0.2 g (2.14 mmol) piperidine were added dropwise and the mixture was stirred under reflux for 6 hours. After cooling to room temperature, stirring was continued overnight. The formed piperidine hydrochloric salt was separated by filtration and the solvent removed with a rotary evaporator. The resulting precipitate containing the crude product was recrystallized with toluene to obtain a dark powder.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07977482B2uspto-grants-2011_07