4-Formylbenzoicacid (1.45 g, 9.66 mmol), DMAP (0.15 g, 1.23 mmol), DCC (2.6 g, 12.60 mmol) and borneol (1.00 g, 6.48 mmol) were added into 30 mL of THF with a calcium chloride drying tube. The reaction was maintained at room temperature for 12 h. Finally, the target product BF with a total yield over 95% was obtained by filtration, evaporation, and further purification with silica gel column chromatography (200−300 mesh; the eluents were petroleum ether: ethyl acetate = 10:1). 1H NMR (JNM-ECA400, JEOL), Fourier transform infrared spectroscopy (FTIR, IR Affinity-1, SHIMADZU) were used to confirm the chemical features of BF, and the results were shown in Figure S12 .
Jnm eca400
Manufactured by JEOL
Sourced in Japan
The JNM-ECA400 is a nuclear magnetic resonance (NMR) spectrometer designed for analytical and research applications. It features a high-field superconducting magnet and advanced electronics to provide precise and reliable measurements of molecular structures and properties.
Automatically generated - may contain errors
Lab products found in correlation
Iraffinity 1, by Shimadzu (1 mentions)
Dsc8230, by Rigaku (1 mentions)
Rid 10a, by Shimadzu (1 mentions)
Atr pro450 s, by Jasco (1 mentions)
Gc 2014, by Shimadzu (1 mentions)
Mcp t610, by Mitsubishi (1 mentions)
Jcm 6000, by JEOL (1 mentions)
Jms 700 spectrometer, by JEOL (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
Kieselgel 60, by Merck Group (1 mentions)
Silica gel, by Merck Group (1 mentions)
6 protocols using jnm eca400
1
Synthesis of Bornyl Formate from 4-Formylbenzoic Acid
2
NMR Spectroscopy of Inclusion Complexes
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All NMR 1H spectra were recorded on JNM-ECA-400 (400 MHz, «JEOL», Tokyo, Japan) NMR spectrometer at the temperature 298 K using DSS (Sodium trimethylsilylpropanesulfonate) as the external standard.
When studying the inclusion complex formation, three types of series were run. One series was prepared in pure deuterated water. Four series were done in a D2O-DMSO-d6 mixed solvent (with DMSO-d6 molar fractions 0.05, 0.075, 0.10 and 0.15) and three series in a D2O-EtOH mixed solvent (with molar fractions of EtOH 0.05, 0.075, and 0.10). In each series, the β-CD concentration held constant (0.0135 mol/L), while the benzoic acid concentration was variable.
When studying the inclusion complex formation, three types of series were run. One series was prepared in pure deuterated water. Four series were done in a D2O-DMSO-d6 mixed solvent (with DMSO-d6 molar fractions 0.05, 0.075, 0.10 and 0.15) and three series in a D2O-EtOH mixed solvent (with molar fractions of EtOH 0.05, 0.075, and 0.10). In each series, the β-CD concentration held constant (0.0135 mol/L), while the benzoic acid concentration was variable.
3
Characterization of Organic Compounds
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All chemicals were reagent grade and were used without further purification except for dichloromethane and triethylamine, which were used after distillation over calcium hydride.
NMR spectra were recorded on a JEOL (Tokyo, Japan) JNM-ECA400 or JNM-ECZ600 FT-NMR spectrometer using residual solvent peak (2.50 ppm for DMSO-d6 and 7.26 ppm for CDCl3) as a reference. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were performed on a Rigaku (Tokyo, Japan) TG8120 instrument. Differential scanning calorimetry (DSC) was performed on a Rigaku (Tokyo, Japan) DSC8230 instrument. Gel permeation chromatography (GPC) was performed using a Shimadzu (Kyoto, Japan) LC-10AT system with a Polymer Laboratories (CA, USA) PolyPore column placed in a Shimadzu (Kyoto, Japan) CTO-10A oven equipped with Shimadzu (Kyoto, Japan) RID-10A and Shimadzu (Kyoto, Japan) SPD-10A detectors.
NMR spectra were recorded on a JEOL (Tokyo, Japan) JNM-ECA400 or JNM-ECZ600 FT-NMR spectrometer using residual solvent peak (2.50 ppm for DMSO-d6 and 7.26 ppm for CDCl3) as a reference. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were performed on a Rigaku (Tokyo, Japan) TG8120 instrument. Differential scanning calorimetry (DSC) was performed on a Rigaku (Tokyo, Japan) DSC8230 instrument. Gel permeation chromatography (GPC) was performed using a Shimadzu (Kyoto, Japan) LC-10AT system with a Polymer Laboratories (CA, USA) PolyPore column placed in a Shimadzu (Kyoto, Japan) CTO-10A oven equipped with Shimadzu (Kyoto, Japan) RID-10A and Shimadzu (Kyoto, Japan) SPD-10A detectors.
4
Comprehensive Material Characterization Protocol
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Gas chromatography (GC) analysis was performed on Shimadzu GC-2014 equipped with FID detector. Fourier transform infrared (FT-IR) was measured by JASCO ATR PRO450-S with Ge. X-ray diffraction (XRD) was measured by PANalytical Co. X’ part PRO using Cu Kα radiation (λ = 1.541 Å) in the 2θ range of 2–75°. The operating tube current and voltage were 40 mA and 40 kV, respectively. The data was collected at the step size of 0.017° and the type of scan was continuous. Energy dispersive X-ray spectroscopy (EDX) was measured by SHIMADZU. Co. Rayny EDX-700HS. The operating tube current and voltage were 100 μA and 15 kV, respectively. Rh was used as X-ray tube. Solid state13 C NMR spectra were obtained by JEOL JNM-ECA400. Scanning electron microscopy (SEM) was performed on the JEOL JSM-6701F scanning electron microscope operating at 5 kV. Freeze-dried of GO was made by using an ADVANTEC DRZ350WC. Electrical conductivity was measured by using MITSUBISHI CHEMICAL ANALYTECH MCP-T610.
5
Multifaceted Characterization of Advanced Materials
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SEM observations were carried out in a SEM JCM-6000 (JEOL) after a 75-second gold sputtering process. High-resolution solid-state NMR analyses were conducted using a JNM-ECA400 (JEOL) at resonance frequencies of 100 MHz for carbon-13. The chemical shift of 13C NMR spectra was determined at room temperatures. GPC measurements were carried out in a JASCO HSS-1500 system with TSK gel α-3000 column (TOSOH) using DMF and LiBr, as solvent. Raman spectroscopies were carried out in a NRS-4100 Laser Raman Spectrometer using laser 532 nm in wavelength. The fracture toughness tests were conducted in an Instron floor machine according to ASTM D5045. The tensile strength and stiffness tests were carried out according to ASTM D638. Creep compliance was measured by means of indentation tests in a Elionix device with a Berkovich diamond tip, by applying a load up to 100 mN at a rate of 2 mN/s, and a holding time at maximum load of 15 seconds.
6
Chromatographic Purification of Compounds
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All reagent-grade chemicals were purchased from Sigma Chemical Co. (St. Louis, MO). The chromatographic separations were carried out by thin-layer chromatography using commercially available glass plates pre-coated with silica gel (E. Merck Co., Darmstadt, Germany) and visualized under UV light at 254 and 360 nm or stained with 10% H 2 SO 4 . Column chromatography was performed on 230-400 mesh silica gel (Kieselgel 60, Merck, Darmstadt, Germany). RP-18 (ODS-A, 12 mm, S-150 A ˚, YMC) and Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Uppsala, Sweden) columns were used for column chromatography. 1 H, 13 C NMR and 2D-NMR data were obtained on a JNM-ECA 400 (Jeol, Tokyo, Japan) spectrometer in CDCl 3 , acetone-d 6 , DMSO-d 6 or methanol-d 4 with tetramethylsilane (TMS) as the internal standard. EIMS and HREIMS data were collected on Jeol JMS-700 spectrometer (JEOL, Tokyo, Japan).
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