Reaktion #2015333

ord-184de579982d4de6aa68cd9ccfe5f073

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturTo a cooled
  2. 2
    SonstigeThe mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane
  3. 3
    workup.ADDITIONwere added
  4. 4
    workup.STIRRINGThe mixture was stirred at room temperature for 1 h
  5. 5
    Filtrationthe precipitate was collected by filtration
  6. 6
    Waschenwashed with water and heptane
  7. 7
    Sonstigedried

Vorschrift

To a cooled and stirred solution of 3′-[4-(4-chloro-phenyl)-6-methyl-pyrimidin-2-yl]-biphenyl-3-sulfonic acid tert-butylamide (0.16 g) in dichloromethane (3 mL) was added TFA (3 mL) and the reaction mixture was allowed to stir at room temperature for 15 h. The mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane were added. The mixture was stirred at room temperature for 1 h, the precipitate was collected by filtration, washed with water and heptane and dried to yield the title compound as an off-white solid (0.083, 63%). MS (ISP) 436.1 [(M+H)+]; mp 221° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08183262B2uspto-grants-2012_05