We added 1.5 mmol of NaNO2 to 1 mmol of MCP dissolved in 3 mL of pre-chilled 18% hydrochloric acid, followed by stirring for 1 hour at 4°C before the addition of sulfamic acid (0.5 mmol). The resulting solution was added to salicylic acid (2 mmol) dissolved in 1 M NaOH (5 mL) and then stirred at 4°C for 1 hour, followed by reaction at room temperature for 6 hours. The pH was adjusted to 9–10 during the reaction. The precipitate was filtered and washed three times with diethyl ether/acetone (1:1) followed by drying in a vacuum oven. The infrared (IR) spectra were recorded on a Varian FT (Fourier transform)-IR spectrophotometer (Varian, Palo Alto, CA, USA). We obtained the proton nuclear magnetic resonance (1H-NMR) imaging spectra by using a Varian AS 500 spectrometer, and the chemical shifts were in ppm downfield from tetramethylsilane. The yield of MCP-azo-ASA was 74%; the melting point (mp) was 132°C–137°C; IR (Nujol mull), νmax (cm−1): 1,627 (C=O, CONH), 1,580 (C=O, COOH); and 1H-NMR (DMSO-d6): δ = 1.16 (t, 6H, J = 6.4 Hz), 2.40–2.49 (m, 6H, overlapped with DMSO-d6 signals), 3.12 (m, 2H), 3.62 (s, 1H), 3.88 (s, 3H), 6.71 (d, 1H, J = 8.4 Hz), 7.21 (s, 1H), 7.75 (dd, J1 = 8.4 Hz, J2 = 2.4 Hz), 7.87 (s, 1H), 8.13 (d, 1H, J = 2.4 Hz), 8.53 (s, 1H), 9.94 (s, 1H).
As 500 spectrometer
Manufactured by Agilent Technologies
Sourced in United States
The AS 500 spectrometer is a high-performance laboratory instrument designed for the analysis of materials. It utilizes spectroscopic techniques to measure and characterize the properties of samples. The core function of the AS 500 is to provide accurate and reliable data on the composition, structure, and behavior of materials under investigation.
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Lab products found in correlation
Silica gel f254, by Merck Group (2 mentions)
Ftir spectrophotometer, by Agilent Technologies (2 mentions)
Esterase, by Merck Group (1 mentions)
Carbonyldiimidazole, by Merck Group (1 mentions)
Dextranase, by Merck Group (1 mentions)
Dimethyl sulfoxide dmso d6, by Cambridge Isotopes (1 mentions)
Varian ft ir spectrophotometer, by Agilent Technologies (1 mentions)
Phosphate buffered saline ph 7, by Thermo Fisher Scientific (1 mentions)
Reaction solvents, by Junsei (1 mentions)
2 4 dinitrobenzenesulfonic acid hydrate, by Merck Group (1 mentions)
Agilent 6530 accurate mass q tof lc ms system, by Agilent Technologies (1 mentions)
5 protocols using as 500 spectrometer
1
Synthesis and Characterization of MCP-azo-ASA
2
Synthesis and Characterization of MTDZ Prodrugs
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Dextran (MW 70,000), dextranase (Penicillium sp.), esterase, 2,4-dinitrosalicylicacid (DNS), succinic anhydride, carbonyldiimidazole (CDI), and MTDZ were obtained from Sigma-Aldrich Chemical Co. (St Louis, MO, USA). Dimethyl sulfoxide (DMSO)-d6 was obtained from Cambridge Isotope Laboratories (Andover, MA, USA). All reagents and solvents for high-performance liquid chromatography (HPLC) were obtained from Merck (Darmstadt, Germany). All other chemicals used were reagent grade, commercially available products. Infrared (IR) spectra were recorded on a Fourier transform-infrared (FT-IR) spectrophotometer (Varian, Palo Alto, CA, USA). 1H-nuclear magnetic resonance (NMR) spectra were obtained using a Varian AS 500 spectrometer, and the chemical shifts were recorded in parts per million (ppm) downfield from tetramethylsilane. Small molecular colon-specific prodrugs of MTDZ, MTDZ sulfate, and NMG were synthesized as described in previous studies.8 (link),9 (link) Structures of the prodrugs are shown in Figure S1 .
3
Synthesis and Characterization of Amino Acid-Based Compounds
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4-PBA, 1,1′-carbonyldiimidazole (CDI), DNBS, L-glutamic acid dimethyl ester hydrochloride, L-aspartic acid dimethyl ester hydrochloride, and sulfasalazine (SSZ) were obtained from Tokyo Kasei Kogyo Co. (Tokyo, Japan). Phosphate-buffered saline (PBS, pH 7.4) was supplied by Thermo Fisher Scientific (Waltham, MA, USA). All organic solvents were purchased from Junsei Chemical Co. (Tokyo, Japan) and used in experiments without further purification. All other chemicals were commercially available products of reagent grade. A Varian FT-IR spectrophotometer (Varian, Palo Alto, CA, USA) and an AS 500 spectrometer (Varian) were used to record infrared (IR) spectra and 1H-NMR spectra, respectively. The chemical shifts in the NMR spectra were reported in ppm, downfield of tetramethylsilane. Elemental analysis was carried out by an Elemental Analyzer System (Profile HV-3, Manchester, UK). Mass analysis was performed using electrospray ionization mass spectrometry (Agilent QQQ 6460 mass spectrometer, Agilent Technologies, Santa Clara, CA, USA).
4
Organic Synthesis of Salicylate Derivatives
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ASP hydrochloride (HCl), salicylic acid, sodium nitrite (NaNO2), sulfamic acid, and 5-ASA were purchased from Tokyo Kasei Kogyo Co. (Tokyo, Japan). SSZ and 2, 4-dinitrobenzenesulfonic acid hydrate (DNBS) were purchased from Sigma Chemical Co. Inc. (St. Louis, MO, USA). Phosphate-buffered saline (pH 7.4, PBS) was purchased from Thermo Fisher Scientific (Waltham, MA, USA). Reaction solvents were obtained from Junsei Chemical Co. (Tokyo, Japan). All other chemicals were reagent grade, commercially available products. Spots on thin-layer chromatography (TLC) plates (silica gel F254s, Merck Millipore, Burlington, MA, USA) were detected using a UV lamp (at 254 nm). IR spectra were recorded using a Varian FT-IR spectrophotometer (Varian, Palo Alto, CA, USA). 1H-NMR spectra were recorded using a Varian AS 500 spectrometer (Varian). The chemical shifts in NMR spectra were reported in ppm downfield from tetramethylsilane.
5
Synthesis and Characterization of Novel Organic Compounds
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Palladium on carbon (Pd/C, 10%) and BT-MA were purchased from Sigma Chemical Co. (St. Louis, MO, USA). TRL, DNBS, NAC, ZnPP, and NaBH4 were purchased from Tokyo Kasei Kogyo Co., Tokyo, Japan. The reaction solvents were obtained from Junsei Chemical Co. (Tokyo, Japan). All other chemicals were of reagent grade and were commercially available. The spots on thin-layer chromatography (TLC) plates (silica gel F254s, Merck Millipore, Burlington, MA, USA) were detected using a 254-nm ultraviolet lamp. Electrospray ionization mass spectrometry (ESI-MS) spectra were obtained using an Agilent 6530 Accurate-Mass Q-TOF LC/MS system (Agilent, Santa Clara, CA, USA). IR and 1H-NMR spectra were recorded using a Varian FT-IR spectrophotometer and a Varian AS 500 spectrometer (Varian, Palo Alto, CA, USA), respectively. The chemical shifts in the NMR spectra were reported in ppm downfield from tetramethylsilane.
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