تفاعل #166652

ord-73db7473352d44a384cd196943dd28cd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated under reduced pressure
  2. 2
    workup.ADDITIONdiluted with DCM and brine
  3. 3
    أخرىThe organic phase was dried
  4. 4
    workup.ADDITION(phase separator silicone treated filter paper)
  5. 5
    أخرىpurified by silica gel chromatography (10-50% ether in DCM)

الإجراء التجريبي

To a solution of 3-iodo-4-nitro-1H-indazole (0.500 g, 1.73 mmol) in DMF (8 mL) was added potassium carbonate (0.478 g, 3.46 mmol) at ambient temperature. After 15 minutes, 2-(chloromethyl)-4-methylthiazole hydrochloride was added. The mixture was allowed to stir at ambient temperature for 18 hours, concentrated under reduced pressure and diluted with DCM and brine. The organic phase was dried (phase separator silicone treated filter paper), and purified by silica gel chromatography (10-50% ether in DCM) to provide 2-((3-iodo-4-nitro-1H-indazol-1-yl)methyl)-4-methylthiazole (0.414 g, 60% yield) as a yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08841455B2uspto-grants-2014_09