commercial suppliers and used without further purification. Reactions
were carried out in 4 mL screw neck glass vials furnished with screw
caps equipped with poly(tetrafluoroethylene) (PTFE)/rubber septa,
and stir bars under ambient atmosphere unless otherwise noted. Silica
gel 60 Å (40–60 μm, 230–400 mesh) was used
for column chromatography. All NMR spectra were recorded in CDCl3 using a Bruker AVANCE II 400 MHz or Bruker Avance 500 MHz.
Chemical shifts are given in ppm relative to the residual solvent
peak (1H NMR: CDCl3 δ 7.26, 13C NMR: CDCl3 δ 77.16) with multiplicity (br = broad,
s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet),
coupling constants (in hertz), and integration. Kinetic data was analyzed
by Agilent 1260 Infinity Quaternary LC (Eclipse Plus 18C column, 3.5
μm, 4.6 × 100 mm2; UV detector, 265 nm) with
a gradient of acetonitrile and 0.1% formic acid in Milli-Q water at
a flow rate of 1 mL/min. The analytes were calibrated using a five-point
calibration curve with threefold dilution between each sample in the
series. HPLC with a chiral stationary phase was performed on an Agilent
1100 series instrument. High-resolution mass spectrometry analyses
were performed by Thermo Scientific Q Exactive HF Hybrid Quadrupole-Orbitrap
HESI or Bruker microTOF ESI, and low-resolution mass analyses by Bruker
Daltonics amaZon speed no 06052 ESI.