Example 1
Commercial-grade reagents and solvents were used without further purification except as indicated. All reactions were stirred magnetically or mechanically shaken; moisture-sensitive reactions were performed under nitrogen atmosphere. Reverse-phase HPLC experiments were conducted with 0.1% aqueous trifluoroacetic acid and 0.1% trifluoroacetic acid in acetonitrile buffers as eluents on C18 reversed-phase columns using a Beckman Coulter HPLC equipped with a System Gold 168 Diode array detector. ESIMS data was obtained on an Agilent 1100 series LC/MSD (XCT) electrospray trap. The microwave reactions were performed in the CEM Discover single-mode reactor with controlled power, temperature, and time settings. The NMR spectra of oxopiperazine compounds were recorded on a Bruker AVANCE 400, 500, or 600 MHz spectrometer.