Tetrahydrofuran soluble

The microautoclave solvent activity tests measure coal conversion in a small batch reactor under carefully controlled conditions. The tests are described as Kinetic, Equilibrium and SRT. The Kinetic and Equilibrium Tests measure coal conversion to tetrahydrofuran solubles at conditions where conversion should be monotonically related to hydrogen transfer. The Kinetic Test is performed at 399°C for 10 minutes at an 8 to 1 solvent to coal ratio. The combination of high solvent ratio and low time provide a measure of performance at essentially constant solvent composition. The measured conversion is thus related to the rate of hydrogen donation from solvent of roughly a single composition. In contrast, the Equilibrium Test is performed at 399°C for 30 minutes at a 2 to 1 solvent to coal ratio. At these conditions, hydrogen donors can be substantially depleted. Thus performance is related to hydrogen donor... 

Pentafluorophenyl)(tetrahydrothiophene)gold(I) is a white crystalline solid, which is air and moisture stable at room temperature. It decomposes before melting (109 °C). It is very soluble in acetone, benzene, dichloromethane, diethyl ether, nitromethane, and tetrahydrofuran, soluble in ethanol and methanol, and insoluble in hexane. 

Mechanism. Under the experimental conditions and concentrations previously described, the addition of Et2AlCl to a chlorobenzene solution of high cw-1,4-polybutadiene, followed by precipitation with methanol, did not reduce the complete hexane or tetrahydrofuran solubility of the polybutadiene. However, when PVC was present during the addition of Et2AlCl to the cw-1,4-polybutadiene, under the same conditions, only 0-40% of the polybutadiene was extractable by hexane, the amount depending upon the reaction time. When the hexane-insoluble residue was extracted with tetrahydrofuran, greater than 90% dissolved. The soluble material was identifiable as unmodified PVC while the hexane-insoluble, tetrahydrofuran-insoluble residue was shown by elemental analysis to contain hydrocarbon residues—i.e., it was a reaction product of PVC and cis-1,4-polybutadiene. When the initially added cw-1,4-polybutadiene... 

The tetrahydrofuran-soluble, butanone-insoluble fraction is reduced in all cases. Where there is no corresponding increase in tetra-hydrofuran-insoluble resin, it is necessary to conclude that Fraction III is reduced by scission to lower molecular weight products. Where the tetrahydrofuran-insoluble resin has increased, Fraction III may, in part, have been insolubilized by crosslinking. 

In Table III are reported elemental analyses of the original sample (toluene-soluble and toluene-insoluble fractions), of the bases obtained from them, and of the unprecipitated remainder. The preasphaltenes, though defined as tetrahydrofuran-soluble, toluene-insoluble materials, are sufficiently soluble in toluene (approximately 1 g/100 mL) to be used in these precipitation experiments. The elemental analysis data suggest that no significant fractionation has taken place in this dissolution step. 

The reaction mixture then was exposed to the atmosphere, and the coal product was isolated. The mixture was centrifuged, and the very dark brown, tetrahydrofuran-soluble material was removed by pipet. Fresh solvent was added to the residue and the mixture was stirred. The mixture then was centrifuged and the soluble material was removed by pipet. This procedure was repeated several times. The final extracts were clear, pale yellow solutions. The combined extracts were filtered through a 1.40-(jim frit. The filtrate was concentrated in vacuo at 50°C to yield a freely flowing, dark brown material (2.252 g). Residual volatile materials were removed in several stages in vacuo. The amount of material present after 2 hr was 1.956 g after 16 hr, 1.678 g after 41 hr, 1.581 g and after 68 hr, 1.521 g. This product is dark brown and does not flow. 

The tetrahydrofuran-soluble portion of the buytlated, C-labeled Illinois No. 6 coal (1.52 g) was chromatographed on silica gel (Baker, 60-200 mesh, 24 g) to remove materials such as the electron transfer agent and the related reduction and alkylation products. These materials were eluted with pure hexane (about 250 mL) and 5 95 tetrahydrofuranihexane (about 250 mL). The dried eluant weighed 0.997 g. The coal products then were eluted with pure tetrahydrofuran (about 250 mL), followed by 50 50 tetrahydrofuran methanol (about 250 mL) and pure methanol (about 250 mL). The dried eluant weighed 0.535 g. The recovery was virtually quantitative. 

Other Alkylation Experiments. In other experiments lithium and sodium were used in place of potassium. Biphenyl and anthracene were used in place of naphthalene. 1,2-Dimethoxyethane was used in place of tetrahydrofuran. Butyl chloride, butyl bromide, butyl mesylate, butyl triflate, methyl iodide, and octyl iodide were used in place of butyl iodide. The conditions used in these experiments were very similar to the conditions used in the procedures described in the previous paragraphs. The isolation procedure was modified in those cases where the ionic salt, e.g., sodium iodide, was soluble in tetrahydrofuran. In these instances the tetrahydrofuran-soluble product was washed with water to remove the salt prior to further study. 

The reaction products were separated into tetrahydrofuran-soluble and tetrahydrofuran-insoluble fractions as already described. The chromatographic separations and spectroscopic investigations also were performed as described. 

The polymers are effective as catalysts of stereoselective hydrogenation of methyl sorbate to c/5-3-hexenoate at 160°C in cyclohexane or tetrahydrofuran. Soluble completes have been isolated after hydrogenation. Then, the catalytic activity decreases this is probably caused by the loss of Cr(CO)3 groups. The results agree with the mechanism involving the dissociation of Cr(CO)3 groups, a considerable amount of which cannot be reassociated with polymeric phenyl groups. 

Tetrahydrofuran soluble magnesium dialkoxides Mg(OR)2 (where R = CPh3 or CMePha) have been prepared" by the reactions of magnesium hydride or dimethyl magnesium with the corresponding alcohols ... 

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