D8 venture instrument

Optical rotations were recorded on a PerkinElmer 241 MC polarimeter
using a 1.0 mL cell. IR spectra were recorded on a PerkinElmer Spectrum One
FT-IR spectrometer. 1D and 2D NMR spectra were recorded with a Bruker Avance 400
MHz instrument at 400 MHz for ¹H NMR and 100 MHz for ¹³C
NMR. Chemical shift values (δ) are given in parts per
million (ppm), and the coupling constants (J) are in hertz
(Hz). All of the chemical shifts were recorded with respect to the deuterated
solvent shift (CDCl₃: δ_H 7.24 for
the proton resonance and δ_C 77.0 for the
carbon, MeOH-d₄:
δ_H 3.31 for the proton resonance and
δ_C 49.1 for the carbon). Both low- and
high-resolution mass spectra were recorded on a Micromass LCT Premier XE mass
spectrometer. X-ray structures were run on a Bruker D8 Venture instrument. All
solvents used were spectral grade or distilled prior to use.

Optical rotations were recorded on a Perkin-Elmer 241 MC Polarimeter using a 1.0 mL cell. IR spectra were recorded on a Perkin Elmer Spectrum One FT-IR spectrometer. Nuclear magnetic resonance (NMR) spectra (1D and 2D) were obtained with a VNMRS Varian 600 MHz, VNMRS Varian 500 MHz, or a Bruker Avance 400 MHz spectrometer. Chemical shift values (δ) were given in parts per million (ppm), and the coupling constants (J) were in Hz. All of the chemical shifts were recorded with respect to the deuterated solvent shift (CDCl₃: δ_H 7.24 for the proton resonance and δ_C 77.0 for the carbon; MeOH-d₄: δ_H 3.31 for the proton resonance and δ_C 49.1 for the carbon; acetone-d₆: δ_H 2.05 for the proton resonance and δ_C 29.92 for the carbon). Mass spectrometry experiments (low and high resolution) were recorded on a Micromass LCT Premier XE Mass Spectrometer. Liquid chromatography/mass spectrometry experiments were run on Agilent 6520 Q-TOF-LC/MS using a Phenomenex Gemini NX-C18 column. The LC was run in a gradient mode from 50% CH₃CN/H₂O with 0.1% formic acid to 100% CH₃CN over 12 minutes, then held at 100% CH₃CN for 3 minutes. X-ray diffraction studies were run on a Bruker D8 Venture instrument. All solvents used were spectral grade or distilled prior to use.