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With ammonium metatungstate hydrate; hydrogen; In water; at 180℃; under 25858.1 - 103432 Torr; for 2h;
Sodium gluconate (10 grams) was combined with 100 mL of water and 2.5 grams, or 2 mol %, of tungstate in the form of ammonium metatungstate hydrate in a 450 cubic Hastelloy C2000 Parr high pressure reactor. The reactor was purged three times with 6.9 MPa (1000 psi) nitrogen, then with 6.9 MPa (1000 psi) hydrogen three times. After the third hydrogen flush, the reactor was pressurized to 3.4 MPa (500 psi) with hydrogen, and stirring at 700 rpm with heating to 180 degrees Celsius was initiated. Once the reaction temperature was reached, additional hydrogen was added to provide 13.8 MPa (2000 psi) of hydrogen to the vessel. After two hours, the reactor contents were cooled to room temperature by quenching in an ice water bath, the reactor was depressurized and the contents filtered to recover the catalyst and then the samples were silylated for GC/MS analysis using N,0-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and trimethylchlorosilane (TMCS) in pyridine. The analysis showed a 91.7 % conversion of the substrate, and products included 15.8 weight percent of 5-hydroxymethyl-2- furancarboxylic acid (HMFCA, 27.4 mol percent yield).
With lithium hydroxide; In water; at 180℃; under 7500.75 Torr; for 2h;Inert atmosphere;
For this example, neither the tungstate or the commercial ruthenium on carbon catalyst were used, and nitrogen was again used in place of hydrogen, except at a pressure of 1.0 MPa (150 psi). Full conversion of the substrate was experienced, with products including 1.29 weight percent of lactic acid (3.4 mol percent yield) of lactic acid, 4.8 weight percent of pyruvic acid (13.11 mol percent yield), and 0.3 weight percent of 5-hydroxymethyl-2-furancarboxylic acid (HMFCA)(4.7 mol percent yield) but no observable glycerol, ethylene glycol or propylene glycol
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