Solid-State Products

A lot of effort, including most of the most recent efforts, involves synthesis of insoluble materials that are characterized using solid-state instrumentation including Raman, IR, MS, solid-state NMR, X-ray and other related instrumentation. Following is a brief review of this effort. 

Self-assembly structures have been reported for lead (IV) and lead(ll) nitrogen-containing hgands, alkoxides, lead(ll) phosphonates, lead(II) phosphinates, and lead(ll) carbonates.  

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Uses. In metallurgy for hardening copper and lead alloys to prepare GaAs for electronic devices, doping agent in germanium and silicon solid state products, special solders. 

To the organic chemist, the most striking feature of solid-state reactions is the stereochemical purity of die product obtained in most cases. This feature allows conversion by conventional methods of the solid-state product to other materials of desired stereochemistries. We illustrate this by some examples of reactions starting from the cyclobutanes obtained by solid-state (2 + 2) photodimerization. 

Pokkuluri et al. have recently addressed the question of the directionality of free volume in their studies on the solid state di-Ti-methane rearrangement of methyl 2-benzoyl-l,4-dihydrol,4-ethenonaphthalene-3-carboxylate, 30 [150]. The title compound gives two different sets of products upon solution and solid state irradiation, both resulting from di-Ti-methane process involving 1,3-diradical intermediate (Scheme 14). Strikingly, the solid state products derive via less stable 1,3-diradical intermediates, 31 and 32 whereas the... 

In AIBN photolysis, as in most solid-state product studies, the reaction was carried out at much higher temperature (200 K), where it is probably safe to assume that steric isotope effects are unimportant. At cryogenic temperatures, however, they should be important whenever strong steric interactions influence the rate of reaction. 

E. Catalano, C.E. Rolon, On The Solid State Products of Thermal Decomposition of Confined and Unconfmed Triaminotrhitrobenzene, Thermochim. Acta, 61 (1983) 37 and 53. 

The need for a multidose formulation may also dictate the use of a solid-state formulation. As the name implies, multidose products are intended to provide the patient with a product that contains several doses of the therapeutic within one container. Multidose formulations contain preservatives to kill any bacteria and prevent mold growth that may result from repeated entry into the drug product. Phenol and benzyl alcohol are two widely used preservatives in protein-based parenteral pharmaceuticals. Frequently, the addition of a preservative to the formulation compromises the long-term stability of the drug product, typically because the protein becomes physically unstable and/or exhibits oxidation. If the formulation scientist can obtain sufficient short-term stability (e.g., 2 weeks) for a formulation containing a preservative, then the use of a solid-state product may enable production of a multiuse formulation. In this case, the preservative is NOT added to the liquid bulk used to prepare the solid state. Instead, when the solid-state formulation is reconstituted prior to use, a preservative is included in the water for reconstitution. Thus the final product to be used is a multidose formulation that will experience only short-term exposure to the preservative. 

The ability to achieve a higher concentration on reconstitution of the solid-state product also may allow the formulation scientist to side-step potential stability-limiting aggregation that may result in a liquid formulation of high-concentration protein. 

Zheng, Z. and Shetty, K. (2000b). Solid state production of polygalacturonase by Lentinus edodes using fruit processing wastes. Process Biochem. 35, 825-830. 

Sankar, G., Wright, P. A., Natarajan, S., Thomas, J. M., Greaves, G. N., Dent, A. J., Dobson, B. R., Ramsdale, C. A., and Jones, R. H. (1993). Combined Quexafs-Xrd a new technique in high-temperature materials chemistry—an illustrative in-situ study of the zinc oxide-enhanced solid-state production of Cordierite from a precursor Zeolite. J. Phys. Chem. 91, 9550-9554. 

Solid-State Production of Polyacetylene from Poly(dietbyl 7-oxabicyclo[2.2.1]hepta-2,5-diene-2,3-dicarboxylate)... 

This may be a rather trivial point, but we still find it important to point out that there are several ways in which molecular or ionic building blocks may be assembled to a solid state product through a solution procedure. 

Conventional techniques used to make these materials consist of a hIgh-temperature furnace, with temperatures ranging from 500°C to 2000°C, to supply the energy needed for the reaction to take place. Because these furnaces may reach only 2000°C, it may take minutes to hours to convert reactants to solid-state products, and the mixtures are heated unevenly. As a result, flaws can be introduced into the structures, which can cause stress points in the materials. 

Modifier for solid-state production of polyethylene terephthalate Netherlands 3,890 1977 Chemische Werke Huels... 

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