반응 #1099225

ord-fa4d49b87a9c492fa7a9777c3bc618ad

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux for 6 hours
  2. 2
    workup.STIRRINGstirring
  3. 3
    기타The formed piperidine hydrochloric salt was separated by filtration
  4. 4
    기타the solvent removed with a rotary evaporator
  5. 5
    workup.ADDITIONThe resulting precipitate containing the crude product
  6. 6
    기타was recrystallized with toluene
  7. 7
    기타to obtain a dark powder

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07977482B2uspto-grants-2011_07