반응 #622796

ord-432221f68edb4850bf7a66283e5b5b6f

용매

반응 조건

온도
160°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with saturated aqueous NaHCO3
  2. 2
    건조dried (Na2SO4)
  3. 3
    여과filtered
  4. 4
    기타chromatographed (0-30% EtOAc/DCM)

실험 절차

A mixture of 4-chlorophthalazin-1(2H)-one (200 mg, 1.11 mmol), sodium 2-methylpropane-2-thiolate (248 mg, 2.22 mmol), tris(trifluoromethylsulfonyloxy)scandium (54.5 mg, 0.11 mmol) and K2CO3 (308 mg, 2.22 mmol) was heated at 160° C. under microwave condition for 30 minutes. The mixture was diluted with EtOAc and washed with saturated aqueous NaHCO3, dried (Na2SO4), filtered, and chromatographed (0-30% EtOAc/DCM) to give 52 mg (20%) of the title compound as a white solid: MS (DCI) 235 (M+H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08859549B2uspto-grants-2014_10