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7 protocols using diethyl ether et2o

1

Synthesis of Epoxy Resin Composites with Organophosphorus Additives

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The epoxy resin Epidian® 601 (EP601) as well as curing agent IDA were purchased from CIECH Resin Sp.z.o.o. (Nowa Sarzyna, Poland). Epidian® 601 is a clear, viscous liquid of light color, epoxy number: 0.500–0.550 mol/100 g, viscosity at 25 °C: 700–1100 mPas, density at 20 °C: 1.140–1.170 g/cm3. The curing agent IDA contains 4,4′-isopropylidenedophenol, an oligomeric reaction product with 1-chloro-2,3-epoxypropane, a reaction product with 3-aminomethyl-3,5,5-trimethylcyclohexylamine, isophorone diamine. Organophosphorus reagents: diethyl chlorophosphate, diphenyl chlorophosphite, and bis(2-ethylhexyl)phosphate was purchased from Sigma-Aldrich (Darmstadt, Germany). The high-purity aluminium oxide hydroxide (boehmite) PURAL SB was made available for our research courtesy of the company Sasol Germany GmbH. Tetrahydrofuran (THF), mesitylene, diethyl ether (Et2O), and chloroform (CHCl3) were purchased from Sigma-Aldrich also. The sodium base, hydrochloric acid, and anhydrous magnesium sulfate come from the company Merck (Darmstadt, Germany). The listed materials were used as received without further purification.
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2

Synthesis of SN-38-PEG-DBCO Conjugate

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All reagents listed below were obtained from
commercial sources and used without further purification. H-His (Trt)-2-Cl-Trt
resin and H-Val-2-Cl-Trt resin were purchased from AAPPTEC (Louisville,
KY). Boc-L-alanine, Fmoc-L-alanine, Nα-Fmoc-Nω-(2,2,4,6,7-pentamethyldihydro-benzofuran-5-sulfonyl)-l-arginine, Nim-Trityl-L-histidine tert-butyl ester
hydrochloride, Fmoc-L-isoleucine, Fmoc-O-tert-butyl-L-tyrosine, Fmoc-L-proline,
Fmoc-6-aminohexanoic acid, 4-aminobenzyl alcohol (PABA), O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium
hexafluorophosphate (HATU),N-ethoxycarbonyl-2-ethoxy-1,2-dihydroquinoline(EEDQ),N,N′-diisopropylethylamine
(DIPEA), trifluoroacetic acid (TFA), and piperidine were purchased
from Chem Impex (Wood Dale, IL). 7-Ethyl-10-hydroxycamptothecin (SN-38)
was purchased from Biosynth (San Diego, CA). N,N-dimethylformamide
(DMF), dichloromethane (DCM), methanol (MeOH), tetrahydrofuran (THF),
acetonitrile (ACN), ethyl acetate (EtOAc), hexane, triisopropylsilane
(TIPS), phosphorus tribromide, diethyl ether (Et2O), silica
gel, 18-crown-6, and potassium carbonate were purchased from Sigma-Aldrich
(Burlington, MA). N3-PEG4-acid, Fmoc-N-amido-PEG3-acid, and DBCO-C6-acid were purchased from BroadPharm
(San Diego, CA).
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3

Synthesis and Characterization of Cadmium Complexes

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The sodium salts of monensin and salinomycin were obtained from Biovet Ltd. (Peshtera, Bulgaria). Tetraethylammonium hydroxide (Et4NOH), nitric acid (HNO3), Cd(II) acetate (Cd(CH3COO)2×2H2O) and diethyl ether (Et2O) were acquired from Merck (Darmstadt, Germany).
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4

Salinomycin Bioavailability Analysis

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Biovet Ltd. (Peshtera, Bulgaria) provided the sodium salt of salinomycin (C42H69O11Na, CAS number: 55721-31-8, purity: >95 %) required for this study. Lead nitrate (Pb(NO3)2), tetraethylammonium hydroxide (Et4NOH) and diethyl ether (Et2O) were purchased from Merck (Darmstadt, Germany). Deferiprone (C7H9NO2, CAS number: 30652-11-0, purity: 98%) was purchased from Sigma Aldrich (St. Louis, MO, USA). HNO3 (≥69%, Rotipuran Supra, Carl Roth, Karlsruhe, Germany) and H2O2 (30%, Suprapur, Merck, Darmstadt, Germany) were used for digestion of the kidneys. All samples were diluted with ultrapure water (18.2 MΩ cm, ELGA water purification system, Purelab Ultra MK 2, UK or 18.2 MΩ cm, Milli-Q Advantage, Darmstadt, Germany). Standard solutions for calibration were purchased from LabKings (Hilversum, The Netherlands).
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5

Synthesis and Characterization of Electrocatalysts

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Graphite powder, Nafion solution (5 wt%), disodium hydrogen phosphate (Na2HPO4), potassium permanganate (KMnO4), sodium tungstate dihydrate (Na2WO4·2H2O), and sodium molybdate dihydrate (Na2MoO4·2H2O) were supplied from Sigma-Aldrich. Methanol (MeOH), hydrochloric acid (HCl), nickel(ii) chloride hexahydrate (NiCl2·6H2O), sulfuric acid (H2SO4), palladium(ii) nitrate dihydrate (Pd[NO3]2·2H2O), ethylene glycol (EG), nitric acid (HNO3), sodium hydroxide (NaOH), diethyl ether (Et2O), isopropyl alcohol (IPA), hydrogen peroxide (H2O2), and sodium nitrate (NaNO3) were purchased from Merck. Commercial Pt/C product (20 wt%, from ETECK) and other chemical materials involved were utilized as received. All chemicals in this investigation were directly used with no more pretreatments. Deionized (DI) water was employed to dilute and dissolve chemical reagents during the experiments.
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6

Peptide Synthesis and Purification Protocol

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A Tribute peptide synthesiser (Protein Technologies, Inc, USA) was utilised to synthesise the mature peptide. After synthesis, the peptide was transferred to a 50-ml round-bottomed flask. Twenty-five ml per gram of mixture cleavage solution (94 % Trifluoroacetic acid (TFA) (Sigma-Aldrich, USA), 2 % dd H2O, 2 % thioanisole (TIS) (Sigma-Aldrich, USA) and 2 % 1–2 ethanedithiol (EDT) (Sigma-Aldrich, USA)) were added into the round-bottomed flask. The round-bottomed flask was stirred with a rotor in the fume hood for 2 h. After cleavage, the mixture solution was filtered by a Buchner funnel, and 3 ml of dichloromethane (DCM) were used to wash (Sigma-Aldrich, USA) three times. Diethyl ether (Et2O) (Aldrich, USA) was added to the mixture to 50 ml in a 50-ml tube. Moreover, the tube was placed at a temperature of −20 °C to precipitate the peptide. After drying in the fume hood, 10 ml of HPLC buffer A (0.5 ml TFA/999.5 ml H2O) were used to dissolve the peptide, and then buffer B (0.5 ml TFA/199.5 ml H2O/800 ml acetonitrile (Sigma-Aldrich, USA)) 5 ml. The tube was put in an Alpha 1–2 LD plus freeze dryer (CHRIST, Germany) for 48–50 h. The dry peptide was then stored at −20 °C, prior to further analyses.
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7

Synthesis of Polyurethane Precursors

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N-Methyldiethanolamine (>99%, Aldrich, Darmstadt, Germany), quinuclidinol-3 (99%, Aldrich, Darmstadt, Germany), 3-aminoquinuclidine dihydrochloride (98%, TCI Europe, Zwijndrecht, Belgium), potassium tetrafluoroborate (99%, Acros, Geel, Belgium), potassium carbonate (K2CO3, > 98%, Aldrich, Darmstadt, Germany), tin(II) 2-ethylhexanoate (98%, Aldrich, Darmstadt, Germany), iodoethane (99%, Aldrich, Darmstadt, Germany), N,N-dimethylformamide (DMF, anhydrous, 99.8%, Acros, Geel, Belgium), dichloromethane (CH2Cl2, anhydrous, 99.8%, Aldrich, Darmstadt, Germany), diethyl ether (Et2O, > 99%, Aldrich, Darmstadt, Germany), acetonitrile (CH3CN, anhydrous, 99.8%, Acros, Geel, Belgium), ethyl acetate (AcOEt, anhydrous, 99.8%, Acros, Geel, Belgium), 1,1,1,3,3,3-hexafluoro-propan-2-ol (HFIP, 99%, Apollo Scientific, Stockport, UK), 4,4′-methylene-bis(cyclohexyl isocyanate) (H12MDI, 2, 99%, Covestro AG, Leverkusen, Germany) and isophorone diisocyanate (IPDI, 3, 98%, Aldrich, Darmstadt, Germany) were used without purification.
Toluene-2,4-diisocyanate (TDI, 1, 95%, Aldrich, Darmstadt, Germany) was purified by vacuum distillation. Meanwhile, 1,5-Dibromopentane (97%, Aldrich, Darmstadt, Germany) and N,N-bis-(3-aminopropyl)methylamine (6, 96%, Aldrich, Darmstadt, Germany) were purified by vacuum distillation over CaH2 and NaOH, respectively.
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