The chemical structure was confirmed via1H-NMR spectroscopy using a BRUKER DPX300NMR spectrometer with tetramethylsilane as an internal standard. Melting points were measured with a Büchi Melting Point B-545.
Dpx 300 nmr spectrometer
Manufactured by Bruker
Sourced in Japan
The DPX-300 NMR spectrometer is a nuclear magnetic resonance (NMR) instrument manufactured by Bruker. It is designed to perform high-resolution NMR spectroscopy analysis. The core function of the DPX-300 is to detect and analyze the magnetic properties of atomic nuclei within a sample to provide information about the chemical structure and composition of the material.
Automatically generated - may contain errors
Lab products found in correlation
Paragon 1000 spectrometer, by Bruker (2 mentions)
Tlc silica gel 60 f254 plate, by Merck Group (2 mentions)
Melting point b 545, by Büchi (1 mentions)
2400 series 2 chn analyzer, by PerkinElmer (1 mentions)
Silica gel g, by Merck Group (1 mentions)
8400s spectrophotometer, by Shimadzu (1 mentions)
Paragon 1000 spectrometer, by PerkinElmer (1 mentions)
Lcms it tof system, by Shimadzu (1 mentions)
9 protocols using dpx 300 nmr spectrometer
1
Characterization of Organic Compounds
2
Comprehensive Characterization of SB-PORPy-COF
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1 H and 13 C NMR were carried out using Bruker DPX-300 NMR spectrometer. Carbon, hydrogen and nitrogen contents of SB-PORPy-COF by Perkin Elmer 2400 Series II CHN analyzer. X-Ray powder diffraction patterns of the samples were obtained with a X'Pert PRO of PANalytical diffractometer using Cu Kα (= 0.15406 nm) radiation. Volumetric Nitrogen adsorption/desorption analysis, Brunauer-Emmett-Teller (BET) specific surface area, pore volume and micropore size etc were carried out at 77 K using Autosorb 1 (quantachrome,USA).
Prior to adsorption measurement the samples were outgassed in vacuum at 150 0 C for 10 h.
NLDFT pore-size distribution was obtained from the adsorption/desorption isotherms by using the carbon/slit-cylindrical pore model. was isolated by solvent evaporation as a yellow solid. The crude was then purified by using flash column chromatography on silica gel (60-120 mesh) using dichloromethane/toluene as an eluent.
The tetra borylated product 2 was isolated as grey solid (1.5 g, yield 76 %).
Mp: >300°C NMR:
Prior to adsorption measurement the samples were outgassed in vacuum at 150 0 C for 10 h.
NLDFT pore-size distribution was obtained from the adsorption/desorption isotherms by using the carbon/slit-cylindrical pore model. was isolated by solvent evaporation as a yellow solid. The crude was then purified by using flash column chromatography on silica gel (60-120 mesh) using dichloromethane/toluene as an eluent.
The tetra borylated product 2 was isolated as grey solid (1.5 g, yield 76 %).
Mp: >300°C NMR:
3
Synthesis and Characterization of FA-CD-PLLD Conjugate
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The dried CD-PLLD (0.76 g, 0.1 mmol) and FA (0.132 mg, 0.3 mmol) were dissolved in 20 mL dried DMF, then 0.3 mmol HOBT and 0.3 mmol HBTU were added. After 48 h reaction at room temperature, the mixture was dialyzed in distilled water for 3 d (MWCO = 3000). The FA-CD-PLLD was obtained by lyophilization with a yield of 68%. Its chemical structure was characterized by lH NMR analyses. The 1H NMR spectra were measured in DMSO-d6 by using a Bruker DPX-300 NMR spectrometer (300 MHz) at 25°C.
4
Spectroscopic Characterization of Pharmaceutical Compounds
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All solvents used were of laboratory grade and were obtained from SD Fine Chemicals (Mumbai, India) and Merck (Mumbai, India). Ciprofloxacin and Ketoconazole were received as gift samples from Dr. Reddys Laboratories, Hyderabad, India. Melting points were determined in open glass capillary tubes and were uncorrected. Compounds were routinely checked for their purity on Silica gel G (Merck) Thin layer chromatography (TLC) plates; iodine chamber and UV lamp were used for visualization of TLC spots. The IR spectra were recorded in KBr pellets on a BIO-RAD FTS FT-IR spectrophotometer. 1H-NMR spectra were recorded on a Bruker DPX-300 NMR spectrometer in CDCl3 using tetramethylsilane (TMS) as an internal standard. The chemical shifts are reported on a ppm scale. Mass spectra were obtained on a JEOL-SX-102 instrument using electron impact ionization. Elemental analyses were performed on a Perkin Elmer model 2400 CHN analyzer and were within ±0.4% of the theoretical values.
5
Dendronized Chitosan Synthesis via Click
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The click reaction between Cs-N3 and PLLD-G3 was carried out as follows: 0.515 g of PLLD-G3 (0.29 mmol) and 0.05 g of Cs-N3 were added successively with magnetic stirring to 10 mL of DMSO. After a clear solution was obtained, 18 mg of CuSO4·5H2O and 28 mg of sodium ascorbate were added successively under a nitrogen atmosphere. The resultant reaction mixture was heated to 40°C for 48 hours. After the reaction, the product was dialyzed in distilled water for 3 days (MWCO =8,000) and lyophilized to obtain the dendronized chitosan derivative (Cs-g-PLLD, yield 73%). FTIR (Perkin–Elmer Paragon 1000 spectrometer) and 1H NMR (Bruker DPX-300 NMR spectrometer) analyses were used to confirm the click reaction between Cs-N3 and PLLD-G3. Based on elemental analysis, the degree of substitution (the number of polyamidoamine dendrons per 100 anhydroglucose units of chitosan) of PLLD-G3 on chitosan was determined to be 10.35.
6
Conjugation of Cs-g-PLLD with Folic Acid
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Conjugation between Cs-g-PLLD and FA was carried out as follows: 10 mL of DMSO, 0.359 g of FA (0.81 mmol), 0.168 g of dicyclohexylcarbodiimide, and 0.102 g of N-hydroxysuccinimde were added successively with magnetic stirring for 5 hours at 25°C. After filtration, a clear solution was obtained, and then, 0.5 mL of solution and 30 mg of Cs-g-PLLD were added successively with magnetic stirring for 48 hours. After the reaction, the product was dialyzed in distilled water for 3 days (MWCO =8,000) and was lyophilized to obtain the dendronized chitosan derivative (Cs-g-PLLD-FA, yield 61%). FTIR (Perkin–Elmer Paragon 1000 spectrometer) and 1H NMR (Bruker DPX-300 NMR spectrometer) analyses were used to confirm this conjugation between Cs-g-PLLD and FA.
7
Synthesis and Characterization of Novel Organic Compounds
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All chemicals were purchased from Sigma-Aldrich Chemical Co. (St. Louis, MO, USA) and Merck KGaA (Darmstadt, Germany). All melting points (m.p.) were determined on an Electrothermal 9100 digital melting point apparatus (Electrothermal, Essex, UK) and are uncorrected. All reactions were monitored by thin-layer chromatography (TLC) using Silica Gel 60 F254 TLC plates (Merck KGaA). Spectroscopic data were recorded with the following instruments: IR: 8400S spectrophotometer (Shimadzu, Tokyo, Japan); 1H-NMR: DPX 300 NMR spectrometer (Bruker Bioscience, Billerica, MA, USA), 13C-NMR: Bruker DPX 75 NMR spectrometer in dimethyl sulfoxide (DMSO)-d6, using TMS as internal standard; HRMS: Shimadzu, Liquid Chromatography/Mass Spectrometer Ion-Trap and Time-of-Flight (LC/MS ITTOF) system.
8
Azido-Modified Chitosan Synthesis
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The introduction of azide groups onto the backbone of chitosan was carried out as follows: 250 mg of chitosan and 180 μL (1.5 mmol) of a freshly prepared solution of 1-azido-2,3-epoxypropane were successively added to distilled water with magnetic stirring. The clear reaction mixture obtained was stirred for 24 hours at 30°C in the dark. After the reaction, the product was dialyzed in distilled water for 3 days (molecular weight cutoff [MWCO] =8,000) and was lyophilized to obtain azido-modified chitosan (Cs-N3, yield 86%). Fourier-transform infrared spectroscopy (FTIR; Perkin–Elmer Paragon 1000 spectrometer; PerkinElmer Inc, Waltham, MA, USA) and 1H nuclear magnetic resonance (NMR; Bruker DPX-300 NMR spectrometer; Bruker Corporation, Billerica, MA, USA) analyses were used to confirm the azidation of amylose by 1-azido-2,3-epoxypropane.
9
Comprehensive Characterization of Organic Compounds
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All chemicals were purchased from Sigma-Aldrich Chemical Co (Sigma-Aldrich Corp., St. Louis, MO, USA) and Merck Chemicals (Merck KGaA, Darmstadt, Germany). All melting points (m.p.) were determined by Electrothermal 9100 digital melting point apparatus (Electrothermal, Essex, UK) and are uncorrected. All the reactions were monitored by thin-layer chromatography (TLC) using Silica Gel 60 F254 TLC plates (Merck KGaA, Darmstadt, Germany). Spectroscopic data were recorded with the following instruments: IR, Shimadzu 8400S spectrophotometer (Shimadzu, Tokyo, Japan); 1H-NMR, Bruker DPX 300 NMR spectrometer (Bruker Bioscience, Billerica, MA, USA), 13C-NMR, Bruker DPX 75 NMR spectrometer (Bruker Bioscience, Billerica, MA, USA) in DMSO-d6, using TMS as the internal standard; M + 1 peaks were determined by Shimadzu LC/MS ITTOF system (Shimadzu, Tokyo, Japan).
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