335 photodiode array detector

Optical rotations were acquired on a Rudolph Research Autopol III polarimeter. NMR experiments used a JEOL ECS-400 (400 MHz for 1H and 100 MHz for 13C; JEOL Ltd., Tokyo, Japan). HRESIMS data were collected with an electrospray ionization source coupled to a Q-ToF Premier mass spectrometer (Waters Corp., Milford, MA, USA) or a LTQ Orbitrap XL system (Thermo Fisher Scientific, San Jose, CA, USA) in positive and/or negative ionization modes by direct injection or via an Acquity UPLC system (Waters Corp.). A CombiFlash Rf 200 system using a RediSep Rf Si-gel Gold column (both from Teledyne-Isco, Lincoln, NE, USA) was employed for normal-phase flash chromatography. HPLC was performed via a ProStar HPLC system with a 335 photodiode array detector (Varian Inc., Palo Alto, CA, USA). YMC ODS-A (Waters Corp.; 5µm; columns of dimensions 250 × 20 mm, 250 × 10 mm, and 150 × 4.6 mm) or Kinetex C18 (Phenomenex; 5µm; columns of dimensions 250 × 21.2 mm and 250 × 4.6 mm) were used for preparative, semi-preparative, and analytical HPLC, respectively. For UPLC analysis, a BEH C18 (Waters Corp.; 1.7 µm; 50 × 2.1 mm) column was used.