Anhydrous dioxane

Manufactured by Thermo Fisher Scientific

Anhydrous dioxane is a clear, colorless organic solvent commonly used in various laboratory applications. It has a high boiling point and is miscible with water and many organic solvents. Anhydrous dioxane is often employed as a reaction medium, extraction solvent, and in the synthesis of organic compounds.

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Lab products found in correlation

Toluene, by Thermo Fisher Scientific (1 mentions) Deuterated methanol, by Thermo Fisher Scientific (1 mentions) Dichloromethane, by Thermo Fisher Scientific (1 mentions) Methanol, by Thermo Fisher Scientific (1 mentions) Hplc grade ammonium acetate, by Thermo Fisher Scientific (1 mentions) Prednisolone, by Steraloids (1 mentions) T butanol, by Thermo Fisher Scientific (1 mentions) Hplc grade acetonitrile, by Thermo Fisher Scientific (1 mentions)

2 protocols using anhydrous dioxane

Steroid Synthesis and Characterization

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All chemicals, reagents, and solvents used
in this synthesis were of reagent grade or better and were inspected
and released for use based on the manufacturer’s Certificates
of Analysis. Prednisolone was from Steraloids, deuterium gas was from
Cambridge Isotopes, Wilkinson’s catalyst was from Combi-Chem,
sodium borohydride was from Oakwood, t-butanol was
from Alfa Aesar, anhydrous dioxane, toluene, dichloromethane, methanol,
and deuterated methanol were from Acros, and all remaining chemicals
and solvents were from Sigma-Aldrich. HPLC analyses used HPLC-grade
acetonitrile (Fisher), HPLC-grade ammonium acetate (Fisher), and deionized
water. For high-resolution LC–MS, water and acetonitrile were
from Fisher (Optima LC/MS grade); ammonium acetate was from Fluka
(LC–MS ultra grade).

Lewin A.H., Hayes J.P., Zhong D., Zhang D., Kormos C.M., Mascarella S.W, & Seltzman H.H. (2023). Isolation of Hemiketal and Hydroxy Ketone Tautomers of Synthetic Intermediates Each Affording 18-Hydroxycortisol-1,6,7-d3. ACS Omega, 8(31), 28185-28195.

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Synthesis of 2,5-Diaminoisophthalic Acid Derivative

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A sample of 500 mg (2.55 mmol) of 2,5-diaminoterephthalic acid (Sigma-Aldrich c/n 717312) was dissolved in 11 mL fresh anhydrous dioxane (Acros Organics) under nitrogen in a stirred three-neck round-bottom flask with a condenser. Next, 0.5 mL (4.18 mmol) of diphosgene was added dropwise, and the flask was heated to 90 °C for 2 h. A second addition of 0.25 mL (2.09 mmol) diphosgene was added dropwise, the temperature increased to 95 °C, and the reaction continued for a further 3 h. The reaction was then chilled to 4 °C in an ice bath, precipitating the product. The precipitate was filtered in a vacuum flask, washed several times with anhydrous diethyl ether, and dried under vacuum at room temperature. Reactions using diphosgene were performed in a well-functioning hood, all waste was neutralized with a saturated sodium bicarbonate solution. The final product was a green solid, 70% yield [¹H NMR: (D6-DMSO) 11.9 (2 NH s), 7.6 (2 ArH s)].

Christy T.W., Giannetti C.A., Houlihan G., Smola M.J., Rice G.M., Wang J., Dokholyan N.V., Laederach A., Holliger P, & Weeks K.M. (2021). Direct mapping of higher-order RNA interactions by SHAPE-JuMP. Biochemistry, 60(25), 1971-1982.

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