Drx 300 mhz spectrometer

d-Glucose and O-phenylene diamine were purchased from Sd-fine, India. Benzaldehyde, dimethyl acetal was purchased from Sigma Aldrich chemicals Pvt. Ltd, USA. Paraldehyde, potassium hydroxide, acetic anhydride, acetic acid and butyraldehyde were purchased from SRL, India. Toluene and ethanol were used after distillation. Column chromatography was performed on silica gel (100–200 mesh). NMR spectra were recorded on a Bruker DRX 300 MHz, spectrometer. Elemental analysis was performed by using PerkinElmer 2400 series CHNS/O analyser. The gels were imaged with a HITACHI-S-3400W Scanning Electron. Thermal transitions for gelators and gels were determined on a NETZSCH DSC 204 instrument. Diffractograms of the dried films were recorded on XRD RINT 2500 diffractometer using Ni filtered Cu Kα radiation X-ray diffractograms of the dried films were recorded on XRD RINT 2500 diffractometer using Ni filtered Cu Kα radiation.

One dimensional NMR was used to confirm the structure and isotopic labeling of the DPM isotopomers. A Bruker DRX 300 MHz spectrometer equipped with a 5 mm broadband probe was used to acquire data. Sample temperature was 25±2°C. Proton spectra were the average of 32 scans (64K points each) acquired over 20 ppm using a 1.0 s recycle delay. The residual water signal was suppressed by presaturation of the HOD resonance. Spectra were processed with 1.0 Hz line broadening, and proton chemical shifts were referenced to 3-(trimethylsilyl) propionate [57] (link). Proton-decoupled carbon spectra were the average of 100 scans (61K points each) acquired over 315 ppm using a 3.0 s recycle delay. Spectra were processed with a 1.5 Hz line broadening, and chemical shifts were referenced indirectly [57] (link). Proton-decoupled phosphorus spectra were the average of 256 scans (64K points each) acquired over 50 ppm using a 6.0 s recycle delay. Spectra were processed with a 3.0 Hz line broadening, and chemical shifts were referenced to phosphocreatine [58] .

Reagents were purchased in the highest available quality from commercial suppliers (Sigma-Aldrich, abcr) and used without further purification. Moisture sensitive reactions were carried out under argon atmosphere. ¹H and ¹³C spectra were recorded on a Bruker DRX 300 MHz spectrometer. Chemical shifts (δ) are reported relative to tetramethylsilane (TMS) referenced to the residual proton signal of the deuterated solvent (DMSO-d₆: 2.50 ppm for ¹H spectra and 39.52 ppm for ¹³C spectra). The following abbreviations were used to denote multiplicities: s = singlet, d = doublet, t = triplet, m = multiplet, and b = broad. Signal assignments are based on ¹H-¹H-COSY, ¹H-¹³C-HSQC, and ¹H-¹³C-HMBC experiments. MS experiments were performed on a Thermo Scientific Q Exactive Orbitrap with an electrospray ion source. Samples were analyzed in the positive ion mode. Reaction control was performed via analytical thin-layer chromatography (TLC, Macherey–Nagel) with fluorescent indicator. Spots were further visualized using cerium molybdate or anisaldehyde staining reagents. Column chromatography was carried out on silica gel 60 (70–230 mesh).

Reagents were purchased in the highest available quality from commercial suppliers (Sigma Aldrich, Acros) and used without further purification. Sodium ¹⁵N-nitrite (98 atom % ¹⁵N) was obtained from Sigma Aldrich. Moisture sensitive reactions were carried out under argon atmosphere. ¹H and ¹³C spectra were recorded on a Bruker DRX 300 MHz spectrometer. Chemical shifts (δ) are reported relative to tetramethylsilane (TMS) referenced to the residual proton signal of the deuterated solvent (DMSO-d₆: 2.50 ppm for ¹H spectra and 39.52 ppm for ¹³C spectra; CDCl₃: 7.26 ppm for ¹H spectra and 77.16 ppm for ¹³C spectra). The following abbreviations were used to denote multiplicities: s singlet, d doublet, t triplet, m multiplet, b broad. Signal assignments are based on ¹H-¹H-COSY and ¹H-¹³C-HSQC experiments. MS experiments were performed on a Finnigan LCQ Advantage MAX ion trap instrumentation (Thermo Fisher Scientific) with an electrospray ion source. Samples were analyzed in the positive- or negative-ion mode. Reaction control was performed via analytical thin-layer chromatography (TLC, Macherey–Nagel) with fluorescent indicator. Spots were further visualized using cerium molybdate or anisaldehyde staining reagents. Column chromatography was carried out on silica gel 60 (70–230 mesh).