Solvents were either distilled over
suitable drying agents or dried using an MBraun SPS (Solvent Purification
System). All experiments were carried out under an inert-gas atmosphere
using standard Schlenk techniques. All chemicals were commercially
available and used without further purification, unless described
otherwise. The 1H, 1H{31P}, 31P{1H}, and 13C{1H} NMR spectra
were recorded at room temperature on Bruker AV400 (at 400, 162, and
100 MHz, respectively) and Bruker DRX500 instruments (at 500, 202,
and 126 MHz, respectively) and calibrated to the residual proton and
carbon signals of the solvent26 (link) or to 85%
H3PO4 externally. High-resolution mass spectra
were recorded on a JEOL AccuTOF GC v 4g, JMS-T100GCV mass spectrometer
(FD) and on a JEOL AccuTOF LC, JMS-T100LP mass spectrometer (CSI).
IR spectra were recorded with a Bruker Alpha-p FT-IR spectrometer
operated in the ATR mode. GC analysis for esters and amides was performed
on a Thermo Scientific Trace GC Ultra equipped with a Restek RTX-200
column (30 m × 0.25 mm × 0.5 μm). Temperature program:
initial temperature 50 °C, hold for 4 min, heat to 130 °C
with 30 °C/min, hold for 2 min, heat to 250 °C with 50 °C/min,
hold for 9 min. Other conditions: inlet temperature 200 °C, split
ratio of 60, 1 mL/min carrier flow, FID temperature 250 °C.
suitable drying agents or dried using an MBraun SPS (Solvent Purification
System). All experiments were carried out under an inert-gas atmosphere
using standard Schlenk techniques. All chemicals were commercially
available and used without further purification, unless described
otherwise. The 1H, 1H{31P}, 31P{1H}, and 13C{1H} NMR spectra
were recorded at room temperature on Bruker AV400 (at 400, 162, and
100 MHz, respectively) and Bruker DRX500 instruments (at 500, 202,
and 126 MHz, respectively) and calibrated to the residual proton and
carbon signals of the solvent26 (link) or to 85%
H3PO4 externally. High-resolution mass spectra
were recorded on a JEOL AccuTOF GC v 4g, JMS-T100GCV mass spectrometer
(FD) and on a JEOL AccuTOF LC, JMS-T100LP mass spectrometer (CSI).
IR spectra were recorded with a Bruker Alpha-p FT-IR spectrometer
operated in the ATR mode. GC analysis for esters and amides was performed
on a Thermo Scientific Trace GC Ultra equipped with a Restek RTX-200
column (30 m × 0.25 mm × 0.5 μm). Temperature program:
initial temperature 50 °C, hold for 4 min, heat to 130 °C
with 30 °C/min, hold for 2 min, heat to 250 °C with 50 °C/min,
hold for 9 min. Other conditions: inlet temperature 200 °C, split
ratio of 60, 1 mL/min carrier flow, FID temperature 250 °C.