Reaktion #1863618

ord-7ccb11801acb43518627983d26c10a8f

Reaktionsbedingungen

Temperatur
5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONIce was added to the suspension
  2. 2
    FiltrationThe suspension was filtered off
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigethe filter cake was dried under vacuo at 50° C.
  5. 5
    Sonstigeto yield 23.0 mg (0.05 mmol, 106%) of the analytically pure target compound

Vorschrift

20.7 mg of 2-[1-(2-fluorobenzyl)-1H-indazol-3-yl]-4-(pyridin-4-ylamino)pyrimidine-5-carbonitrile (31-1, 0.049 mmol, 1 eq.) were added to ice bath cooled conc. sulfuric acid (1.84 mmol, 37.5 eq.) and stirred for five minutes at 5° C. and further 24 hours at room temperature. Ice was added to the suspension. The suspension was filtered off, washed with water and the filter cake was dried under vacuo at 50° C. to yield 23.0 mg (0.05 mmol, 106%) of the analytically pure target compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09265763B2uspto-grants-2016_02