Ddr spectrometer

¹H NMR spectra were recorded at 25 °C on a Varian (Varian, Palo Alto, California, United States) DDR spectrometer (599.9 MHz for ¹H) equipped with a dual 5 mm inverse detection gradient (IDPFG) probe-head with z-gradient. ¹H NMR spectra were collected in 32,000 data points using 32 scans with a spectral window of 6000 Hz and referenced to the methanol (fenbufen solutions) or the methanol-d₄ (fenoprofen solutions) signals. For the suppression of the water signal, the double pulse field gradient spin echo (DPFGSE) sequence was used.
The 2D ROESY spectrum of the fenoprofen-BCyD 1:5 complex was recorded at 25 °C using Bruker (Bruker, Billerica, Massachusetts, United States) Avance III spectrometer (700.1 MHz for 1H) equipped with a 5 mm inverse TCI probehead with z-gradient. The Bruker rosygpph19 pulse sequence was used with a mixing time of 300 ms and a spectral width of 10 ppm in both dimensions. The spectrum was acquired into 1024 complex points in t2 with 128 scans coadded at each of 256 t1 increments. The spectrum was processed to 2048 × 1024 data points.

NMR spectra of the isolated compounds were recorded in methanol-d₄ or DMSO-d₆ at 25 °C on a Varian DDR spectrometer (599.9 MHz for 1H and 150.9 MHz for 13C) equipped with a dual 5 mm inverse detection gradient (IDPFG) probe head. Standard pulse sequences and parameters were used to obtain 1D 1H, and various 2D COSY, [1H-13C] HSQC, and [1H-13C] HMBC spectra. Chemical shifts were referenced relative to the solvent resonances.

One-dimensional ¹H and 2D ROESY NMR spectra of the fenbufen–BCyD (4 mM fenbufen, 8 mM BCyD in D₂O dissolved with small amount of NaOD) and nimesulide–BCyD (2 mM nimesulide, 6 mM BCyD in D₂O dissolved with small amount of NaOD) complexes were recorded at 25 °C on a Varian DDR spectrometer (599.9 MHz for ¹H, Varian, Palo Alto, CA, USA) equipped with a dual 5 mm inverse detection gradient (IDPFG) probe head with z-gradient. All spectra were processed using MestReNova 14.2, Mestrelab Research, Santiago de Compostela, Spain. ROESY spectra were measured using the ROESYAD pulse sequence with a mixing time of 300 ms and a spectral width of 10 ppm in both dimensions. The spectrum was acquired into 901 complex points in t2 with 32 scans coadded at each of 256 t1 increments. The spectrum was processed to 1024 × 2048 data points.
NMR measurements of fenoprofen were provided in a previous, closely related article [22 (link)].