- Azelanitrile preparation method
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The invention relates to an azelanitrile preparation method, which comprises: (1) dissolving glutaraldehyde in a solvent, adding a condensation catalyst and an optional cocatalyst, adding cyanoaceticacid in batches to maintain the temperature of the reaction solution of not more than 40 DEG C, and carrying out a condensation reaction, wherein a molar ratio of the glutaraldehyde to the cyanoaceticacid is 1:2; and (2) further adding a palladium carbon catalyst (Pd/C) to the condensation reaction liquid obtained in the step (1), introducing hydrogen gas, maintaining the pressure, heating, and carrying out a decarboxylation and hydrogenation reaction to obtain azelanitrile, wherein the hydrogen pressure is 3.0-4.0 MPa. According to the present invention, the method can perform the reaction by using the one-step method so as to eliminate the separation and purification process of the intermediate product, such that the reaction process is simple, and the cost is low.
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- Odd-even effect in melting properties of 12 alkane-α,ω-diamides
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Fusion and solid-to-solid transitions of a homologous series of 12 linear alkane-α,ω-diamides H2NCO-(CH2)(n-2)-CONH2, where n = (2 to 12 and 14), were investigated by differential scanning calorimetry (d.s.c.). The temperatures of fusion of even terms decreased from Tfus ≈ 572 K to about 460 K, whereas those of odd terms remained substantially constant at about 450 K. Solid-to-solid transitions were also detected for oxamide, malonamide, succinamide, adipamide, suberamide, and dodecanediamide. Regular odd-even alternation was displayed by the temperature, enthalpy, and entropy of fusion values, terms with even number of carbon atoms showing higher values than odd terms. This behaviour was attributed to different crystal packing allowing consonance between hydrogen bonding and dispersive interaction in even terms, which are characterised by multilayer structure, whereas in odd terms a strained three-dimensional network results in looser packing. Parallel alternation of densities in solid alkane-α,ω-diamides supports this interpretation. Comparison was made with literature values for temperatures, enthalpies, and entropies of fusion of isoelectronic linear alkanes, dicarboxylic acids, and alkyldiamines.
- Badea, Elena,Gatta, Giuseppe Della,D'Angelo, Domenico,Brunetti, Bruno,Reckova, Zuzana
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p. 1546 - 1552
(2008/02/11)
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- Selective conversion of nitriles to amides by Amberlyst A-26 supported hydroperoxide
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A mild, efficient and selective conversion of nitriles to amides is achieved by employing Amberlyst A-26 supported hydroperoxide, which is prepared in situ from hydrogen peroxide and Amberlyst A-26 (OH- form). Nitriles and dinitriles are transformed to their corresponding amides and diamides, respectively. Reactions proceed within 0.5-5 hr upon addition of a catalytic amount of Amberlyst A 26(OH-) to a methanolic solution of nitrile and hydrogen peroxide (35%), at room temperature.
- Mansour Lakouraj,Bahrami
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p. 974 - 975
(2007/10/03)
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