As shown in Figure 8 A, the SPc was synthesized according to the method described by Li et al. [9 (link)]. In brief, the SPc was synthesized using the commercial and cheap material sources through two reaction steps. The 2-bromo-2-methylpropionyl bromide (253 mg, 1.11 mmol) was added dropwise into the pentaerythritol solution (25 mg, 0.18 mmol) in dry tetrahydrofuran (THF, 20 mL) and triethylamine (TEA, 111.3 mg, 1.11 mmol) at 0°C. The reaction was quenched with methanol after stirring for 24 h at room temperature, and the product was recrystallized in cold ether to obtain the star initiator Pt-Br (50 mg, 40%) that was confirmed by 1H NMR (CDCl3, Bruker 400, Billerica, Massachusetts, USA). The Pt-Br (40 mg, 0.055 mmol), DMAEMA (2.2 g, 7.7 mmol) and dry THF (8 mL) were added into a flask, and the mixture was degassed by nitrogen for 30 min. The CuBr (46 mg, 0.22 mmol) and PMDETA (110 mg, 0.44 mmol) were then added, and the polymerization was carried out at 60 °C for 7 h. The reaction was quenched by cooling and air exposure, and the THF was removed and recycled for the next polymerization to decrease the production cost. The crude polymer was purified by dialysis in water four times, and the white powder of SPc was finally obtained, which was also confirmed by 1H NMR (CDCl3, Bruker 400, Billerica, MA, USA).
Cdcl3
Manufactured by Bruker
Sourced in United States, Germany
CDCl3 is a deuterated chloroform solvent commonly used in nuclear magnetic resonance (NMR) spectroscopy. It serves as a standard reference for 1H and 13C NMR experiments, providing a stable and well-characterized signal for calibration and signal assignment.
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Lab products found in correlation
Linear polystyrene standards, by Waters Corporation (2 mentions)
Spectrum two ft ir spectrometer, by PerkinElmer (1 mentions)
Amazon sl spectrometer, by Bruker (1 mentions)
Poloxamer f127, by Merck Group (1 mentions)
Peg ppg peg, by Merck Group (1 mentions)
Spectrofluorometer, by Jasco (1 mentions)
V 570 spectrophotometer, by Jasco (1 mentions)
Avance 3 500 nmr spectrometer, by Bruker (1 mentions)
Fp 6500, by Jasco (1 mentions)
Ft ir 6300 spectrophotometer, by Jasco (1 mentions)
Rft600 spectrophotometer, by Jasco (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
Kieselgel 60h, by Merck Group (1 mentions)
Sephadex lh 20, by Merck Group (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Seveneasy ph meter, by Mettler Toledo (1 mentions)
Silica gel 60 pf254 cards, by Merck Group (1 mentions)
Jms hx110 spectrometer, by JEOL (1 mentions)
Melting point b 540 apparatus, by Büchi (1 mentions)
Kieselgel 60, by Merck Group (1 mentions)
17 protocols using cdcl3
1
Synthesis of Pentaerythritol-based Star Polymer
2
Synthesis of N,N-di(2-pyridyl)-N',N'-di(4-pyridyl)-1,4-phenylenediamine
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Example 3
A mixture of 2,2′-dipyridylamine (5.27 g, 30.76 mmol), (4-bromophenyl)-di(4-pyridyl)amine (2.50 g, 7.69 mmol), anhydrous potassium carbonate (2.66 g, 19.23 mmol), bronze powder (4.93 g, 77.64 mmol), 18-crown-6 (200 mg, 0.76 mmol), and DMF (125 mL) was heated at 145 degrees C. under nitrogen for 30 hours. The reaction was cooled and worked up by a procedure similar to that for L1. A yellowish solid was collected from a silica gel column, and was further purified by recrystallization from dichloromethane and petroleum ether, to afford a white solid of N,N-di(2-pyridyl)-N′,N′-di(4-pyridyl)-1,4-phenylenediamine (L2, 1.32 g, yield: 41%). 1H NMR (CDCl3, Bruker 400 MHz): 8.43 (d, J=4.4 Hz, 4H, pyridyl-H), 8.37 (d, J=3.6 Hz, 2H, pyridyl-H), 7.60-7.65 (m, 2H, pyridyl-H), 7.21 (d, J=8.8 Hz, 2H, phenylene-H), 7.14 (d, J=8.8 Hz, 2H, phenylene-H), 6.98-7.09 (m, 8H, pyridyl-H). Anal. Calcd (%) for C26H20N6: C, 74.98; H, 4.84; N, 20.18. Found: C, 74.53; H, 4.72; N, 19.89. IR (KBr pellet, cm−1): 1575(vs), 1505(s), 1490(s), 1467(s), 1431(vs), 1324(s), 1305.13(s), 1276(s), 1218(m), 1163(w), 1103(w), 991(m), 811(m), 777(m), 737(w), 654(w), 622(m), 530(m).
3
Characterization of Organic Compounds
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The reagents and solvents used in this work were obtained from Fluka, Sigma-Aldrich or Merck and used without further purification. Melting points were determined on a Stuart SMP3 and were uncorrected. The infrared spectroscopy (IR) was performed on a Perkin-Elmer FT-IR Spectrometer Spectrum Two with KBr. NMR spectra were recorded in CDCl3, at 500 MHz (Bruker). Chemical shifts were reported in parts per million (δ) using the residual solvent signals (CDCl3: δH 7.26, δC 77.16) as internal standards for 1H and 13C NMR spectra and coupling constants (J) are reported in Hz. Mass spectra were acquired using IT-MS Bruker AmaZon SL spectrometer. TLC was performed on silica gel Merck 60 F254 and TLC plates were visualized by spraying with phosphomolybdic acid reagent and heating.
4
Synthesis of PLA-PEG Block Copolymers
5
Characterization of Organometallic Compounds
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IR spectra (4000–400 cm–1) and far-IR spectra (680–150 cm–1) were acquired as KBr pellets using a JASCO FT/IR-6300 spectrophotometer and as CsI pellets using a JASCO FT/IR 6700 spectrophotometer (JASCO, Tokyo, Japan), respectively. Raman spectra (4000–200 cm–1) were obtained on solid powders employing a JASCO RFT600 spectrophotometer fitted with a YAG laser 600 mW (JASCO, Tokyo, Japan). 1H-NMR (500 MHz) spectra were obtained on a Bruker AVANCE III-500 NMR spectrometer at room temperature (298 K) in CDCl3 as solvent (Bruker Japan, Yokohama, Japan). 1H chemical shifts were reported as δ values relative to residual chloroform. UV-Vis spectra (solution and solid, 800–200 nm) were recorded on a JASCO V-570 spectrophotometer (JASCO, Tokyo, Japan). The values of ε were calculated per metal(I) ion. Mulls for spectroscopy were prepared by finely grinding microcrystalline material into powders with a mortar and pestle and then adding mulling agents (nujol, poly(dimethylsiloxane), viscosity 10,000). Fluorescence spectra were acquired on a JASCO FP-6500 (solid, 700–300 nm) spectrofluorometer (JASCO, Tokyo, Japan). Absorption and luminescence spectra were recorded using solid samples cooled with a liquid nitrogen cryostat (CoolSpeK USP-203, Unisoku Scientific Instruments, Osaka, Japan). Elemental analyses were performed at the Department of Chemistry, University of Tsukuba.
6
Structural Analysis of mPEG-DC Polymer
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1H-NMR spectra of the polymer in CDCl3 (300 MHz NMR spectrometer, Bruker, USA) were used to determine the structure of the mPEG-DC. 1H-NMR spectra of the mPEG-DC in D2O were compared to confirm the core-shell structure of the polymer in water.
7
Echinochrome A Isolation and Characterization
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Drug substance echinochrome A and drug product Histochrome were produced by G.B. Elyakov Pacific Institute of Bioorganic Chemistry (Vladivostok, Russia). TSKgel Toyopearl HW-40 (TOYO SODA, Tokyo, Japan), and Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Uppsala, Sweden) were used for column chromatography. HPLC-grade water and acetic acid were purchased from Panreac Quimica (Barcelona, Spain). MeCN grade 0 was sourced from Cryochrom (Saint Petersburg, Russia). Other solvents used in this study were of analytical grade. Deuterated solvents acetone-d6, CDCl3, CD3CN, and Bruker® SampleJet NMR tubes WIMWG10007SJ (178 mm, cap, O.D. 5.0 mm) for NMR experiments were purchased from Sigma (St. Louis, MO, USA).
8
NMR and GPC Analysis of PBLA-Polyureas
9
Analytical Techniques for Natural Product Isolation
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NMR spectra in deuterated chloroform were captured using a Bruker (400 MHz) instrument (CDCl3). Buchi Rotavapor performed the solvent evaporation (Essen, Germany). Vacuum Liquid Chromatography (VLC) and Gel Permeation Chromatography (GPC) were both carried out using Kieselgel 60H and Sephadex LH 20 (Sigma-Aldrich, St. Louis, Missouri, USA), respectively. Precoated thin layer chromatography plates were used for the compound analysis (Silica gel 60 F 254, Merck, Germany). The spots on the TLC plates were seen using UV light and vanillin/H2SO4 reagents. The remainder of the reagents and solvents were all analytical-grade and bought from a reputable supplier (Active Fine Chemicals Ltd., Bangladesh; Merck, Germany; DaeJung, Korea). The source for vincristine sulfate and butylated hydroxy anisole was Opsonin Pharma Ltd., Dhaka, Bangladesh.
10
Polymer Characterization by NMR, GPC, and pH Titration
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Polymer structure was characterized by nuclear magnetic resonance (NMR) spectroscopy via 1H NMR in CDCl3 (Bruker 500 MHz) and analyzed using TopSpin 3.5 software. Polymer molecular weight was characterized by gel permeation chromatography (GPC); polymers were dissolved in butylated hydroxytoluene–stabilized tetrahydrofuran with 5% DMSO and 1% piperidine, filtered through a 0.2-μm polytetrafluoroethylene filter, and characterized using GPC against linear polystyrene standards (Waters, Milford, MA). pH titrations were performed using a SevenEasy pH meter (Mettler Toledo) with 10 mg of polymer dissolved in 10 ml of 100 mM NaCl acidified with HCl, as previously described (15 (link)). Polymer was titrated from pH 3.0 to 11.0 using 100 mM NaOH added stepwise, and pH was recorded after each addition.
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