Method of Oxidization Using Nitric Acid
a technology of nitric acid and oxidizing method, which is applied in the field of oxidizing method using nitric acid, to achieve the effect of reducing thermal control problems, improving product isolation, and being readily availabl
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example 1
General Methods
[0031]Solutions were concentrated in vacuo (10-15 mbar) using a rotary evaporator and water bath at 50° C. pH measurements were made with a Thermo Orion 310 pH meter (Thermo Fisher Scientific, Inc., Waltham, Mass., USA) which was calibrated prior to use. Oxidations were carried out in Mettler Toledo Labmax reactor. The Labmax reactor is designed to operate as a computer controlled closed-system reactor. The Labmax was fitted with a top-loading balance, a liquid feed pump, an oxygen Sierra flow valve, a mechanically driven stirring rod, a thermometer, a 1 liter thermal jacketed flask, a FTS recirculating chiller, a pressure manifold fitted with pressure relief valves and pressure gauge and a personal computer with CamileTG v1.2 software. The software installed allows the operator to program experiments based on specific parameters and conditions.
example 2
Nitric Acid Oxidation of D-Glucose
[0032]The aqueous 62.3% D-glucose solution used in the oxidations was prepared by adding solid D-glucose (162.5 g, 0.75 mol) to 97.5 grams of deionized water in a screw-capped flask containing a stir bar. Prior to adding solid D-glucose to the water, the water was heated to ca. 60° C. with stirring. Once the D-glucose was dissolved, the temperature was reduced to ambient and dry sodium nitrite (0.60 g) added to the solution. The total weight of the solution is 260.6 g.
[0033]The Recipe Menu is accessed using the Labmax CamileTG v1.2 software and the reaction parameters for the oxidation were programmed in a series of stages: Stage 1—the reactor temperature was set at 25° C.; the stirring rod speed set at 200 rpm (and held constant throughout all the remaining stages); time set for 1 minute. Stage 2—the reactor temperature was set at 25° C., and the pressure set at 0.25 bar for a duration of 3 minutes. Stage 3—the temperature of the reactor was set at...
example 3
Nitric Acid Oxidation of D-Glucose
[0037]The oxidation of D-glucose was carried out as in Example 1. However, potassium hydroxide was substituted for sodium hydroxide in the neutralization process to give crude D-glucaric acid dipotassium salt (151.25 g, 70.4% based on pure dipotassium D-glucarate). The salt was precipitated from methanol as described to give an off white solid (145.75 g, 67.9% based on pure dipotassium D-glucarate).
[0038]Monopotassium D-glucarate isolation, Method 1. D-Glucose (162.5 g, 0.75 mol) was oxidized using the LabMax reactor and concentrated as described. The concentrate of organic product(s) and residual nitric acid was diluted with deionized water (150 mL) and chilled at 5° C. for 18 h. The pH of the solution was adjusted to a constant pH of 9.1 with 45% KOH (184 mL) in an ice bath and the solution back-titrated to pH 3.4 with concentrated HNO3 (34.6 mL) in an ice bath. A precipitate formed when the solution pH dropped below 5. After cooling the mixture a...
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