Reaktion #166704

ord-f4f16e6457164f6688e4c6f5ef7da4b7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction was then concentrated to dryness
  2. 2
    workup.DISSOLUTIONdissolved in minimal DCM
  3. 3
    workup.ADDITIONadded dropwise to a stirring solution of 1M HCl in ether
  4. 4
    FiltrationThe solid product was filtered
  5. 5
    Waschenwashed with ether
  6. 6
    Sonstigedried

Vorschrift

(R)-tert-Butyl 2-(4-(5-bromo-1H-pyrrolo[2,3-b]pyridin-4-yl)piperazin-1-yl)-1-cyclohexyl-2-oxoethylcarbamate (0.010 g, 0.019 mmol) was placed in DCM (3 mL) at room temperature. TFA (0.3 mL) was then added. The reaction was stirred at room temperature for 1 hour. The reaction was then concentrated to dryness, dissolved in minimal DCM, and added dropwise to a stirring solution of 1M HCl in ether. The solid product was filtered, washed with ether, and dried to give (R)-2-amino-1-(4-(5-bromo-1H-pyrrolo[2,3-b]pyri din-4-yl)piperazin-1-yl)-2-cyclohexylethanone (0.005 g, 62% yield) as the dihydrochloride salt. MS ESI (+) m/z 421 detected.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841304B2uspto-grants-2014_09