Neutral alumina

Manufactured by Thermo Fisher Scientific

Neutral alumina is an inert, granular solid material commonly used as a adsorbent and desiccant in various laboratory applications. It is characterized by a high surface area, good thermal stability, and low reactivity.

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5 protocols using neutral alumina

Electrochemical Synthesis of TMTTF Salt

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50 mg of (n-Bu₄N)₂Ta₂F₁₀O were dissolved in 12 mL of dichloromethane passed through neutral alumina from Acros. This solution was divided into two parts of 6 mL each. Then, 5 mg of TMTTF were added in one of it and sonicated for 5 minutes. The two solutions were poured into an electrocrystallization cell, so that the cathodic compartment contained only the supporting electrolyte, and the anodic one both the supporting electrolyte and the TMTTF donor. The two chambers were degassed with argon. Crystals of the salt were grown at 20 °C over a period of 1 week on a platinum wire electrode, diameter 1 mm, by applying a constant current of 1 μA. Thick black shiny plates were obtained on the anode.

Mroweh N., Mézière C., Allain M., Auban-Senzier P., Canadell E, & Avarvari N. (2020). Conservation of structural arrangements and 3 : 1 stoichiometry in a series of crystalline conductors of TMTTF, TMTSF, BEDT-TTF, and chiral DM-EDT-TTF with the oxo-bis[pentafluorotantalate(v)] dianion. Chemical Science, 11(37), 10078-10091.

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Synthesis of Organic Charge-Transfer Salt Crystals

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30 mg of (n-Bu₄N)₂Ta₂F₁₀O were dissolved in 12 mL of dichloromethane passed through neutral alumina from Acros. This solution was divided into two parts of 6 mL each. Then, 5 mg of TMTSF were added in one of it and sonicated for 5 minutes. The two solutions were poured into an electrocrystallization cell, so that the cathodic compartment contained only the supporting electrolyte, and the anodic one both the supporting electrolyte and the TMTSF donor. The two chambers were degassed with argon. Crystals of the salt were grown at 20 °C over a period of 1 week on a platinum wire electrode, diameter 1 mm, by applying a constant current of 1 μA. Thick black plates were obtained on the anode and in the solution.

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Electrocrystallization of BEDT-TTF salt

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60 mg of (n-Bu₄N)₂Ta₂F₁₀O were dissolved in 12 mL of dichloromethane passed through neutral alumina from Acros. This solution was divided into two parts of 6 mL each. Then, 5 mg of BEDT-TTF were added in one of it and sonicated for 10 minutes. The two solutions were poured into an electrocrystallization cell, so that the cathodic compartment contained only the supporting electrolyte, and the anodic one both the supporting electrolyte and the BEDT-TTF donor. The two chambers were degassed with argon. Crystals of the salt were grown at 20 °C over a period of 1 week on a platinum wire electrode, diameter 1 mm, by applying a constant current of 0.5 μA. Thick black shiny plates were obtained on the anode.

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Ruthenium(II) Complexes Synthesis and Characterization

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All materials were used as received without further purification unless otherwise noted. Diethyl ether, acetone, acetonitrile, and methanol were procured from Fisher Scientific, and dichloromethane was obtained from Macron Fine Chemicals. N,N-Dimethylformamide was purchased from Sigma-Aldrich and was dried under nitrogen by passing through a column of activated alumina. Reineke salt, ammonium hexafluorophosphate, lithium chloride, sodium chloride, sodium acetate trihydrate, ascorbic acid, 1,3-diphenylisobenzofuran (DPBF), acetylacetonate, 1,10-phenanthroline, 4,4′-dimethylbipyridyl, acetonitrile-d₃ and acetone-d₆ were purchased from Sigma-Aldrich, and 2,2′-bipyridine was obtained from Alfa Aesar. Sulfuric acid and sodium bicarbonate were received from Fisher Scientific, and potassium ferrioxalate was purchased from Strem Chemicals. Neutral alumina was purchased from Fisher Scientific. The starting material [Ru(p-cymene)Cl₂]₂,21 (link) and the complexes [Ru(p-cymene)(bpy)Cl]Cl, [Ru(p-cymene)(4,4′-Me₂bpy)Cl]Cl, [Ru(p-cymene)(phen)Cl]Cl, and Ru(p-cymene)(acac)Cl were synthesized according to published procedures.21b

Al-Afyouni M.H., Rohrabaugh TN J.r., Al-Afyouni K.F, & Turro C. (2018). New Ru(ii) photocages operative with near-IR light: new platform for drug delivery in the PDT window †Electronic supplementary information (ESI) available. CCDC 1841086–1841088. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c8sc02094a. Chemical Science, 9(32), 6711-6720.

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Synthesis of Silicone-based Surfactants

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Gluconolactone, d-maltose monohydrate, lactobionic acid, cysteamine hydrochloride, and 2,2-dimethoxy-2-phenylacetophenone (DMPA) were purchased from Sigma Aldrich. Pentamethyldisiloxane (PMDS), bis(trimethylsiloxy)-methylsilane (BisH), vinyltrimethoxysilane, vinyltris(trimethylsiloxy)methylsilane (V1), and MCS-V212 (V4) were purchased from Gelest. Iodine was purchased from Anachemia, and potassium hydroxide and sodium bicarbonate were obtained from Caledon Laboratories. All compounds were used as received. Solvents methanol, ethanol, 2-propanol, hexane, dichloromethane, and toluene were also purchased from Caledon and dried through an activated alumina column as needed. Anhydrous methanol, deuterated chloroform (CDCl₃), and deuterated DMSO-d₆ were purchased from Sigma Aldrich and used as received. Neutral alumina was purchased from Fisher Chemical. A Celite S filter aid and Amberlite IR120, hydrogen form, the latter rinsed with distilled water before use, were purchased from Sigma Aldrich. Silsurf J1015-O and Silsurf A008-up were a gift from Siltech Corporation. Silwet L-7657 was purchased from Momentive. n-Wet and o-Wet were provided by EnRoute Interfaces, Inc.
Compounds V2,V3, and V1–V4 → CV1–CV4 have previously been reported [1 (link)]. We include, below, the preparation of V2 and conversion to CV2 to illustrate the simplicity of the process.

Lusterio A, & Brook M.A. (2021). Naturally Derived Silicone Surfactants Based on Saccharides and Cysteamine. Molecules, 26(16), 4802.

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