Reaktion #1752307

ord-cdda95f52c83490e8e801965d992bd69

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solution is evaporated under vacuum
  2. 2
    workup.DISSOLUTIONredissolved in DMSO (0.5 ml)
  3. 3
    Sonstigepurified by mass-directed preparative HPLC
  4. 4
    SonstigeThe purified fractions are evaporated under vacuum

Vorschrift

3-(4-Isobutoxy-piperidine-1-sulfonyl)-benzoic acid (0.03 mmol, 10.2 mg) is treated with a solution of HATU (11.4 mg, 0.03 mmol) in DMF (1 ml) followed by a solution of 3,5-Diamino-6-chloro-pyrazine-2-carboxylic acid [1,3,8-triaza-spiro[4.5]dec-(2E)-ylidene]-amide dihydrochloride (Ex. 38) (11.9 mg, 0.03 mmol) and N-methyl morpholine (0.010 ml, 0.03 mmol) in DMF (1 ml) and shaken at room temperature overnight. The solution is evaporated under vacuum, redissolved in DMSO (0.5 ml) and purified by mass-directed preparative HPLC. The purified fractions are evaporated under vacuum to afford the title compound; [M+H]+ 648.4

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08039472B2uspto-grants-2011_10