Reaktion #2366329

ord-56cd254cec764f38bd8b8a163f730d8f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe volatiles were removed in vacuo
  2. 2
    SonstigeThe residue was purified by preparative HPLC (C18 column, acetonitrile/water gradient)

Vorschrift

1320 mg of the crude (2-{4-[6-(4-Methoxymethoxy-phenyl)-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-4-ylmethyl]-2,2,5,5-tetramethyl-piperazin-1-yl}-ethyl)-methyl-carbamic acid tert-butyl ester were dissolved in 6 ml of 1,4-dioxane and treated with 4 ml of hydrochloric acid (4M in dry dioxane). After standing at rt for 1.5 h the volatiles were removed in vacuo. The residue was purified by preparative HPLC (C18 column, acetonitrile/water gradient) and 45 mg (5%) of the title compound were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09133181B2uspto-grants-2015_09