1h nmr

Manufactured by Bruker

Sourced in Germany, United States, Switzerland

The 1H NMR (Proton Nuclear Magnetic Resonance) is a laboratory instrument used to analyze the structure and composition of chemical compounds. It detects and measures the resonance of hydrogen nuclei (protons) within a sample when exposed to a strong magnetic field and radio waves. The 1H NMR provides information about the chemical environment and connectivity of hydrogen atoms within a molecule, which is essential for the identification and characterization of organic and inorganic compounds.

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Lab products found in correlation

29si nmr spectroscopy, by Bruker (3 mentions) Y1 20, by Shin-Etsu Chemical (3 mentions) Nicolet 6700, by Thermo Fisher Scientific (3 mentions) 13c nmr, by Bruker (2 mentions) 13c nmr spectroscopy, by Bruker (1 mentions) Fe sem, by Zeiss (1 mentions) Ftir spectroscopy, by Bruker (1 mentions) Phosphate buffered saline (pbs), by Thermo Fisher Scientific (1 mentions) Gelatin, by Merck Group (1 mentions) Agilent 8860, by Agilent Technologies (1 mentions) Frontier ir, by PerkinElmer (1 mentions) Nicolet is10 ftir, by Thermo Fisher Scientific (1 mentions) Waters breeze hplc system, by Waters Corporation (1 mentions) Dc alufolien kieselgel 60 f254, by Merck Group (1 mentions) Tlc silica gel plates, by Anatech (1 mentions) 2414 refractive index detector, by Waters Corporation (1 mentions) Ultrahydrogel 250 column, by Waters Corporation (1 mentions) 1525 hplc pump, by Waters Corporation (1 mentions) Mass spectrometry, by Bruker (1 mentions) 13c nmr 100 mhz, by Bruker (1 mentions)

64 protocols using 1h nmr

Synthesis of Silicone Resin Compound

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Example 5

Into a 3 L flask equipped with a stirrer, a thermometer, a nitrogen inflow instrument, and a reflux condenser, 135.5 g (0.25 mol) of a compound shown by the formula (S-1), 28.5 g (0.05 mol) of a compound shown by the formula (S-3b), and 86.0 g (0.2 mol) of a compound shown by the formula (S-7) were introduced. Then, 2,000 g of toluene was added thereto, and the mixture was heated to 70° C. Subsequently, 1.0 g of toluene solution of chloroplatinic acid (platinum concentration of 0.5% by mass) was introduced, and 58.2 g (0.30 mol) of a compound shown by the formula (S-5) and 604.0 g (0.20 mol) of a compound shown by the formula (S-6) (y=40) were added dropwise over 1 hour (total molar number of the hydrosilyl groups/total molar number of the alkenyl groups=1/1, silicone content: 69.0% by mass; when the molar number “f” of S-3b was assumed to be 1, d=4, c+e=5, and g=0). After completion of the dropwise addition, the mixture was heated to 100° C. and aged for 6 hours. Then, toluene was evaporated from the reaction solution under reduced pressure to give a product with a weight average molecular weight of 43,000 measured by GPC in terms of polystyrene. The obtained resin was defined as Resin (5), and was used for Examples. Incidentally, the obtained resin was determined as the resin shown by the general formula (1) by ¹H NMR (product of Bruker Corporation).

US10451970B2. Silicone skeleton-containing polymer, photo-curable resin composition, photo-curable dry film, laminate, and patterning process (2019-10-22). SHIN-ETSU CHEMICAL CO., LTD. [JP]. Inventors: Hitoshi Maruyama [JP], Kazunori Kondo [JP], Michihiro Sugo [JP].

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Synthesis of Silicone Resin (7)

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Example 7

Into a 3 L flask equipped with a stirrer, a thermometer, a nitrogen inflow instrument, and a reflux condenser, 108.4 g (0.20 mol) of a compound shown by the formula (S-1), 53.0 g (0.20 mol) of a compound shown by the formula (S-2), and 57.0 g (0.10 mol) of a compound shown by the formula (S-3a) were introduced. Then, 2,000 g of toluene was added thereto, and the mixture was heated to 70° C. Subsequently, 1.0 g of toluene solution of chloroplatinic acid (platinum concentration of 0.5% by mass) was introduced, and 58.2 g (0.30 mol) of a compound shown by the formula (S-5) and 604.0 g (0.20 mol) of a compound shown by the formula (S-6) (y=40) were added dropwise over 1 hour (total molar number of the hydrosilyl groups/total molar number of the alkenyl groups=1/1, silicone content: 68.6% by mass; when the molar number “f” of S-3a was assumed to be 1, d=0, c+e=4, and g=0). After completion of the dropwise addition, the mixture was heated to 100° C. and aged for 6 hours. Then, toluene was evaporated from the reaction solution under reduced pressure to give a product with a weight average molecular weight of 43,000 measured by GPC in terms of polystyrene. The obtained resin was defined as Resin (7), and was used for Examples. Incidentally, the obtained resin was determined as the resin shown by the general formula (1) by ¹H NMR (product of Bruker Corporation).

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Synthesis of a Silicone Resin Polymer

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Example 3

Into a 3 L flask equipped with a stirrer, a thermometer, a nitrogen inflow instrument, and a reflux condenser, 53.0 g (0.20 mol) of a compound shown by the formula (S-2), 57.0 g (0.10 mol) of a compound shown by the formula (S-3a), and 86.0 g (0.20 mol) of a compound shown by the formula (S-7) were introduced. Then, 2,000 g of toluene was added thereto, and the mixture was heated to 70° C. Subsequently, 1.0 g of toluene solution of chloroplatinic acid (platinum concentration of 0.5% by mass) was introduced, and 58.2 g (0.30 mol) of a compound shown by the formula (S-5) and 604.0 g (0.20 mol) of a compound shown by the formula (S-6) (y=40) were added dropwise over 1 hour (total molar number of the hydrosilyl groups/total molar number of the alkenyl groups=1/1, silicone content: 70.4% by mass; when the molar number “f” of S-3a was assumed to be 1, d=2, c+e=2, and g=0). After completion of the dropwise addition, the mixture was heated to 100° C. and aged for 6 hours. Then, toluene was evaporated from the reaction solution under reduced pressure to give a product with a weight average molecular weight of 44,000 measured by GPC in terms of polystyrene. The obtained resin was defined as Resin (3), and was used for Examples. Incidentally, the obtained resin was determined as the resin shown by the general formula (1) by ¹H NMR (product of Bruker Corporation).

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Synthesis of Resin A from Benzoxazole

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Example 4

Synthesis of Resin A

A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 325.0 g (0.5 mol) of benzoxazole compound S-1a and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 755.0 g (0.25 mol) of the compound having formula (S-2) wherein d=40 (Shin-Etsu Chemical Co., Ltd.) and 48.5 g (0.25 mol) of the compound having formula (S-4) (Shin-Etsu Chemical Co., Ltd.) were added dropwise over 1 hour. The molar ratio of the total amount of hydrosilyl groups to the total amount of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin A. On ¹H-NMR and ²⁹Si-NMR (Bruker Corp.) spectroscopy, Resin A was identified to comprise repeating units of formulae (1a) and (1b). Resin A had a Mw of 42,000 and a silicone content of 67.0 wt %. In formulae (1a) and (1b), a=0.5 and b=0.5.

US10538630B2. Silicone-modified polybenzoxazole resin and making method (2020-01-21). Shin-Etsu Chemical Co., Ltd. [JP]. Inventors: Hitoshi Maruyama [JP], Ryuto Hayashi [JP], Kazunori Kondo [JP], Hideyoshi Yanagisawa [JP].

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Synthesis of Silicone-Based Resin 6

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Example 6

Synthesis of Resin 6

A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 39.2 g (0.10 mol) of Compound (S-1), 26.5 g (0.10 mol) of Compound (S-2), 27.1 g (0.05 mol) of Compound (S-3c), 9.3 g (0.05 mol) of Compound (S-4), and 86.0 g (0.20 mol) of Compound (S-7), further with 2,000 g of toluene, and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 58.2 g (0.30 mol) of Compound (S-5) and 317.0 g (0.20 mol) of Compound (S-6) wherein y¹=20 (Shin-Etsu Chemical Co., Ltd.) were added dropwise over 1 hour. The molar ratio of the total amount of hydrosilyl groups to the total amount of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 6. On ¹H—NMR and ²⁹Si—NMR spectroscopy (Bruker Corp.), Resin 6 was identified to contain recurring units having formulae (a1) to (a5) and (b1) to (b5). On GPC analysis, it was confirmed that the peaks assigned to the reactants had disappeared, proving that a polymer corresponding to the charge ratio was synthesized. Resin 6 had a Mw of 44,000 and a silicone content of 56.3 wt %.

US11402756B2. Silicone structure-containing polymer, photosensitive resin composition, photosensitive resin coating, photosensitive dry film, laminate, and pattern forming process (2022-08-02). Shin-Etsu Chemical Co., Ltd. [JP]. Inventors: Hitoshi Maruyama [JP], Kazunori Kondo [JP].

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Synthesis of Resin 4 via Hydrosilylation

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Example 4

Synthesis of Resin 4

A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 39.2 g (0.10 mol) of Compound (S-1), 26.5 g (0.10 mol) of Compound (S-2), 32.5 g (0.05 mol) of Compound (S-3a), 9.3 g (0.05 mol) of Compound (S-4), and 86.0 g (0.20 mol) of Compound (S-7), further with 2,000 g of toluene, and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 58.2 g (0.30 mol) of Compound (S-5) and 317.0 g (0.20 mol) of Compound (S-6) wherein y¹=20 (Shin-Etsu Chemical Co., Ltd.) were added dropwise over 1 hour. The molar ratio of the total amount of hydrosilyl groups to the total amount of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 4. On ¹H—NMR and ²⁹Si—NMR spectroscopy (Bruker Corp.), Resin 4 was identified to contain recurring units having formulae (a1) to (a5) and (b1) to (b5). On GPC analysis, it was confirmed that the peaks assigned to the reactants had disappeared, proving that a polymer corresponding to the charge ratio was synthesized. Resin 4 had a Mw of 43,000 and a silicone content of 55.7 wt %.

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Nanogel Crosslinking Characterization

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¹H NMR (Bruker, 400 MHz) was conducted on nanogels to determine the extent of intermolecular double bond conversion following UV irradiation. Spectra of a 10 wt% solution of nanogels in CDCl₃ with 1.0 wt% DMPA were obtained, and the NMR tube was exposed to the same irradiation conditions as described in the coating formation. This procedure was repeated for nanogel solutions that also contained 10 wt% mercaptoethanol. Post-reaction spectra of the same samples were obtained immediately following irradiation.

Dailing E.A., Nair D.P., Setterberg W.K., Kyburz K.A., Yang C., D’Ovidio T., Anseth K.S, & Stansbury J.W. (2015). Combined, Independent Small Molecule Release and Shape Memory via Nanogel-Coated Thiourethane Polymer Networks. Polymer chemistry, 7(4), 816-825.

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Synthesis of Poly(methacryloyloxyethyl phosphorylcholine)

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MPC (5.08 g, 17.2 mmol), CPD (47.5 mg, 0.170 mmol), and V-501 (19.1 mg, 0.0681 mmol) (mole ratio 100:1:0.4) were dissolved in a water/methanol solvent (17.0 mL, 9/1, v/v). The solution was purged with argon gas, stirring for 30 min to remove the oxygen. After that, the solution was heated at 70 °C for 4 h. The monomer conversion was 98.5%, as estimated from proton nuclear magnetic resonance (¹H NMR, Bruker, Billerica, MA, USA) before purification (Figure S1). The reaction mixture was dialyzed against pure water for one day. The polymer (PMPC) was recovered by a freeze-drying technique (4.34 g, 85.4%). The values of the number-average molecular weight (M_n(GPC)) and the molecular weight distribution (M_w/M_n), as estimated from gel-permeation chromatography (GPC, Tosoh Co. Tokyo, Japan) measurements were 27.9 kDa and 1.37, respectively. The degree of polymerization calculated from ¹H NMR (DP(NMR)) was 98.

Fukumoto H., Ishihara K, & Yusa S.I. (2021). Thermo-Responsive Behavior of Mixed Aqueous Solution of Hydrophilic Polymer with Pendant Phosphorylcholine Group and Poly(Acrylic Acid). Polymers, 13(1), 148.

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Synthesis of PEG2000-Hyd-PEI1.8K Conjugate

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First, 1 g PEG2000-NH₂ was dissolved in 10 mL chloroform to obtain PEG2000-Hyd-OH. Subsequently, HO-Hyd-COOH (1.1 eq.), EDC (2.0 eq.), and DMAP (0.1 eq.) were added, and the reaction was performed at RT for 8 h. The reaction solution was concentrated through vacuum rotary evaporation, precipitated in a large amount of glacial ether, filtered, collected, and then subjected to vacuum drying. The resulting PEG2000-Hyd-OH (1 g) was dissolved in 10 mL ultra-dry acetonitrile supplemented with di(p-nitrophenyl) carbonate (1.0 eq.) and triethylamine (5.0 eq.), and then reacted at 50 °C for 5 h. Following that, a PEI (1.0 eq.) solution dissolved in 5 mL chloroform was added and the mixture was reacted at RT for 0.5 h. After removing the solvent through vacuum rotary evaporation, 5 mL methanol was added to dissolve the product, which was then placed in a dialysis bag (MW: 2000) and dialyzed in pure water for 24 h. The dialysate was collected and freeze-dried to obtain PEG2000-Hyd-PEI1.8 K. The molecular structure of PEG2000-Hyd-PEI was determined using ¹H-NMR (400 MHz, Bruker, Germany).

Xia Y., Zhang Y., Du Y., Wang Z., Cheng L, & Du Z. (2024). Comprehensive dry eye therapy: overcoming ocular surface barrier and combating inflammation, oxidation, and mitochondrial damage. Journal of Nanobiotechnology, 22, 233.

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Synthesis of DSPE-PEG2000-SS31 Conjugate

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First, DSPE-PEG2k-NHS (100 mg) was dissolved in 3 ml DMF. For complete dissolution, the SS-31 peptide (1.1 equivalents) and triethylamine (3.0 equivalents) were added, and the reaction was conducted at Room Temperature (RT) for 12 h. Subsequently, the reaction solution was transferred to a dialysis bag (MW: 2000 Da) and dialyzed in pure water for 24 h. The dialysate was then collected and freeze-dried to obtain DSPE-PEG2000-SS31. Finally, the molecular structure of DSPE-PEG2000-SS31 was identified using ¹H-NMR (400 MHz, Bruker, Germany).

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