2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol tetra p-toluenesulfonate has been synthesized from nitromethane via condensation, cyclization, oxidative coupling, hydrolysis, and sulfonation. The total yield was 46.5 %. The structures of the title compound and intermediates were characterized by 1H NMR, IR, and MS. X-ray single-crystal diffraction analysis revealed the title compound belongs to triclinic system; the space group is P-1. Mr = 856.89. The crystal cell data were: a = 11.341(2) nm, b = 13.743(3) nm, c = 14.845(3) nm, α = 104.69(3)°, β = 98.80(3)°, γ = 110.30(3)°, V = 2023.7(9) nm3, Z = 2, Dc = 1.406 g cm−3, F(000) = 892, μ = 0.306 mm−1, R = 0.0749, and wR 2 = 0.1893. Results from study of the thermal properties of the compound by DSC indicated its melting point and decomposition temperature were 400.25 and 510.70 K, respectively.
Research on Chemical Intermediates – Springer Journals
Published: Aug 2, 2013
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