Hydrogen in solid phase

JM Schlatter, RH Mazur, O Goodmonson. Hydrogenation in solid phase peptide synthesis. I. Removal of product from the resin. Tetrahedron Lett 2851, 1977. 

Normatov, I. (1992) Role of hydrogen in solid-phase synthesis reaction of cadmium sulfide, Journal of Inorganic Materials 28(8), 1800-1802. 

Khan SA, Sivanandaiah KM. Catal)4ic transfer hydrogenation in solid-phase peptide synthesis synthesis of bradykinin. Synthesis 1978 10 750-751. 

Carbon increases slightly the solubility of hydrogen in solid phase [1965Sch] and decreases its solubihty in liquid phase [1981Sch]. Under 0.1 MPa of hydrogen pressure at 1600°C, the hydrogen solubihty goes from 1.9 10 mol% for pure iron to 0.6 10 mol% for a hquid of composition FcsC. 

Multicomponent reaction systems are highly valued in solid-phase organic synthesis because several elements of diversity can be introduced in a single transformation.1 The Mannich reaction is a classic example of a three-component system in which an active hydrogen component, such as a terminal alkyne, undergoes condensation with the putative imine species formed from the condensation of an amine with an aldehyde.2 The resultant Mannich adducts contain at least three potential sites for diversification specifically, each individual component—the amine, aldehyde, and alkyne—can be varied in structure and thus provide an element of diversity. 

JW van Nispen, JP Polderdijk, WPA Janssen, HM Greven. Replacement of hydrogen fluoride in solid phase peptide synthesis by methanesulfonic acid. Rec Trav Chim Pays-Bas 100, 435, 1981. 

In the liquid-phase procedure the reduced iminoaza peptide 52 is readily obtained by catalytic hydrogenation of the -CH=N- bond of the corresponding iminoaza peptide 41 (Scheme 20). In solid-phase synthesis the reduction of the iminoaza peptide is performed by NaBH3CN. As shown in Scheme 19 reduction by NaBH3CN of compound 48 followed by acidolytic treatment gives the reduced iminoaza peptide 51. 

Direct hydrogenation of C60 in solid phase is carried out at pressure 50-80 MPa and temperatures 573-623 K (Goldshleger and Moravskii 1997). The equilibrium pressures of hydrogen in the reactions (Fig. 4.14)... 

The hydride generation ICP-mass spectrometric technique [75] had a sensitivity of 6.4 ng/g selenium in plant material and was applied to digests of corn, kale and rice. In the isotope dilution mass spectrometric technique [77], the samples were spiked with 76-selenium solution and digested on a heating block at 150 °C with a mixture of nitric acid and hydrogen peroxide. Solid-phase microextraction was used to extract selenium from plant material prior to the gas chromatographic techniques [76]. See also Sects. 7.34.1 and 7.34.2. 

Z.A. Matysina and D.V. Schur, Hydrogen and solid phase transformations in metals, alloys andfullerites (in Russian). (Izd. Nauka i obrazovanie, Dnepropetrovsk, 2002). 

As an explanation of the process of macroradicai decay the mechanism of radical state migration by means of hydrogen atoms elimination from adjacent chains has been suggested and confirmed. The activation energies of various macroradicai reactions have been measured and found to be very high. This is due to a specifity of the kinetic process in solid phase and to the participation of the diffusion phenomenon. Comparative investigation of the reactivity of various macroradicals reveals a great importance of the steric factor, i. e. the entropy ot the transition state for the kinetics of macroradicai reactions. 

The related o-bromobenzyl carbonates have been developed for use in solid-phase peptide synthesis. An aryl o-bromobenzyl carbonate is stable to acidic cleavage (CF3CO2H) of a f-butyl carbamate a benzyl carbonate is cleaved. The o-bromo derivative is quantitatively cleaved with hydrogen fluoride (0°C, 10 min). ... 

The storage of hydrogen in solid-solution materials is characterized by endothermic and exothermic phase change reactions. The thermodynamic nature of these reactions requires the full characterization of influential material properties to enable the optimization of heat and mass transfer within the system. Additionally, the thermodynamic nature of the materials will define the containment technologies required to withstand the operational pressures and temperatures. 

The analysis of NMR spectra of high resolution in solid phase as well as the results of mass-spectrometry investigation of water and methanol desorption from trimethylsilylated aerosil surface with no OH-groups [64,115] testify a nonhydroxylic nature of the sites of adsorption of small water amounts. A correspondence has been fixed of three characteristic regions of the sorbed water and methanol elimination with desorption maxima related to probable destruction of hydrogen-bonded (low-temperature maximum) and coordinate adsorption complexes of various structure (high-temperature maximum) by the help of desorption-field mass-spectrometry [116,117]. 

Bur] Burylev, B.P., Solubility of Hydrogen in Solid Iron Alloys , Russ. J. Phys. Chem., 40(4), 442-445 (1966) (Phase Relations, Calculation, 12)... 

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