Réaction #304470

ord-60fa658fa8d2456994805c4053daaea4

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Filtrationthe precipitate was collected by filtration
  2. 2
    workup.STIRRINGstirred at room temperature for 3 hours
  3. 3
    FiltrationThe insoluble material was collected by filtration
  4. 4
    Lavagewashed with methylene chloride
  5. 5
    Autredried under reduced pressure

Mode opératoire

m-Chloroperbenzoic acid (7.10 g, 31.9 mmol) was added to a solution of 4-(5-chloro-6-cyano-1H,3H benzo[de]isochromen-6-yl)-6-methylsulfamyl-[1,3,5]triazin-2-ylamine (10.0 g, 29.0 mmol) in methylene chloride (100 mL) at room temperature. After the reaction solution was stirred at room temperature for 15 hours, the precipitate was collected by filtration. The resulting precipitate was suspended in methylene chloride, and stirred at room temperature for 3 hours. The insoluble material was collected by filtration, washed with methylene chloride, and dried under reduced pressure. The title compound was obtained as light brown solid (8.34 g, 79%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08193351B2uspto-grants-2012_06