NMR spectra were recorded on Varian Mercury
Plus 300 (299.97 MHz for 1H, 75.44 MHz for 13C, and 282.23 MHz for 19F) or Agilent 400-MR DDR2 (399.94
MHz for 1H, 100.58 MHz for 13C, and 376.29 MHz
for 19F) at 298 K unless otherwise indicated. Chemical
shifts δ are given in parts per million, using residual solvent
as an internal standard. 19F NMR and 31P NMR
chemical shifts were measured relative to CCl3F and H3PO4, respectively. Coupling constants J are reported in hertz. High-resolution mass spectra were obtained
on Q-Tof Micro (Waters), equipped with a quadrupole, TOF analyzers,
and an MCP detector or LTQ Orbitrap Velos (Thermo Fisher Scientific).
Gas chromatography–mass spectrometry (GC–MS) spectra
were obtained on GC–MS DSQ II (Thermo). Thin layer chromatography
analyses were carried out on DC Alufolien Kieselgel 60 F254 (Merck).
Preparative column chromatography separations were performed on silica
gel Kieselgel 60 of 0.040–0.063 mm (Merck). Melting points
were measured on a Boetius melting point apparatus and are uncorrected.
Starting materials, reagents, and substrates were obtained from commercial
suppliers and used without further purification. The solvents were
purified and dried using standard procedures. For synthesis of reagents,
see theSupporting Information .
Plus 300 (299.97 MHz for 1H, 75.44 MHz for 13C, and 282.23 MHz for 19F) or Agilent 400-MR DDR2 (399.94
MHz for 1H, 100.58 MHz for 13C, and 376.29 MHz
for 19F) at 298 K unless otherwise indicated. Chemical
shifts δ are given in parts per million, using residual solvent
as an internal standard. 19F NMR and 31P NMR
chemical shifts were measured relative to CCl3F and H3PO4, respectively. Coupling constants J are reported in hertz. High-resolution mass spectra were obtained
on Q-Tof Micro (Waters), equipped with a quadrupole, TOF analyzers,
and an MCP detector or LTQ Orbitrap Velos (Thermo Fisher Scientific).
Gas chromatography–mass spectrometry (GC–MS) spectra
were obtained on GC–MS DSQ II (Thermo). Thin layer chromatography
analyses were carried out on DC Alufolien Kieselgel 60 F254 (Merck).
Preparative column chromatography separations were performed on silica
gel Kieselgel 60 of 0.040–0.063 mm (Merck). Melting points
were measured on a Boetius melting point apparatus and are uncorrected.
Starting materials, reagents, and substrates were obtained from commercial
suppliers and used without further purification. The solvents were
purified and dried using standard procedures. For synthesis of reagents,
see the