Reaktion #86534

ord-a8466ab727434df4ba6107e6e03447d3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux under nitrogen overnight
  3. 3
    SonstigeThe mixture was evaporated
  4. 4
    Sonstigethe resultant residue was purified on RP-HPLC (XBridge C18 Column
  5. 5
    Wascheneluting with a gradient of acetonitrile/water containing 0.15% NH4OH)
  6. 6
    Sonstigeto give the product as the free base

Vorschrift

A mixture of 6-bromo-9H-purine (0.064 g, 0.32 mmol), 7-(1-aminoethyl)-3-methyl-6-pyridin-4-yl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one (0.046 g, 0.16 mmol), and N,N-diisopropylethylamine (0.056 mL, 0.32 mmol) in ethanol (0.5 mL) was heated at reflux under nitrogen overnight. The mixture was evaporated and the resultant residue was purified on RP-HPLC (XBridge C18 Column, eluting with a gradient of acetonitrile/water containing 0.15% NH4OH) to give the product as the free base. LCMS calculated for C19H17N8OS (M+H)+: m/z=405.1. Found: 405.1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434746B2uspto-grants-2016_09