Mx 2080 32

Optical rotations were measured on a JASCO P-2000 at the D-double emission line of Na°. UV-vis spectra were measured on a JASCO V-630 spectrometer. FTIR spectra were collected on thin-film samples using a JASCO FTIR-4100 fitted with an ATR accessory (ZnSe plate). 1D NMR and inverse-detected 2D NMR spectra were measured on a Bruker Avance II NMR spectrometer with a 1.7 mm¹H{¹³C/¹⁵N} 600 MHz microcryoprobe. Other NMR spectra were measured on a JEOL ECA spectrometer equipped with a 5 mm¹H{¹³C} 500 MHz room-temperature probe.¹³C NMR spectra were measured using a Varian NMR spectrometer equipped with a 5 mm Xsens¹³C{¹H} 125 MHz cryoprobe. NMR spectra are referenced to residual solvent signals. High-resolution ESITOF analysis was carried out on an Agilent 1200 HPLC coupled to an Agilent 6230 TOFMS. Low-resolution MALDI MS measurements were made on a Bruker Biflex IV in a nitrobenzyl alcohol matrix. Low-resolution MS measurements were made on a Thermoelectron Accela UHPLC coupled to an MSQ single-quadrupole detector. Preparative, semi­preparative, and analytical HPLC were performed on a JASCO PU-2086 Plus system consisting of a dynamic mixer (MX-2080–32) with UV-VIS detector (UV-2075) operating at λ 250 nm. Automated flash chromatography was carried out with a Teledyne-Isco CombiFlash system with UV (λ 250 nm) and RI detection.