Method of producing reduced coenzyme q10 as oily product
A reduced type, coenzyme technology, applied in organic chemistry, quinone separation/purification, etc., to achieve the effect of reducing operation time and reaction time
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[0149] Further illustrate the present invention below, but these examples in no way have any limitation to the scope of the present invention, in this example, reduced coenzyme Q 10 Purity and Reduced Coenzyme Q 10 / oxidized coenzyme Q 10 The weight ratio of is determined by the specific HPLC analysis described below. However, the measured reduced coenzyme Q 10 The purity of is by no means a limitation on the purity values obtained in accordance with the present invention. Similarly, the resulting reduced coenzyme Q 10 / oxidized coenzyme Q 10 The weight ratio value does not represent the upper limit of the ratio.
[0150] (Conditions of HPLC) column: SYMMETRY C18 column (product of Waters Company), 250mm (length), 4.6mm (inner diameter); Mobile phase: ethanol: methanol=4: 3 (v / v); Detection wavelength: 210nm; Flow rate: 1ml / min; reduced coenzyme Q 10 Retention time: 9.1min; oxidized coenzyme Q 10 Retention time: 13.3min.
example 1
[0152] oxidized coenzyme Q 10 (100 g; purity 99.4%) was stirred and melted at 50°C. When stirring (power required for stirring: 0.3kw / m 3 ), the prepared aqueous solution is gradually added to the oily product, and the reduction reaction is carried out at 50° C. and a pH value of 4 to 6. The aqueous solution is 100 g of sodium dithionite (purity: at least 75%) dissolved in Prepared in 1000ml of water. After two hours, stir (power required for stirring: 0.3kw / m 3 ), and the mixture was cooled to 2° C. to obtain a white crystalline slurry (flowable crystalline slurry is better). All the above operations were done under nitrogen atmosphere. The obtained crystalline slurry was filtered under reduced pressure, and the wet crystals were rinsed sequentially with cold water and cold ethanol (the temperature of the cold solvent used for washing was 2° C.), and then the wet crystals were dried under reduced pressure (20 to 40° C., 1 to 30 mmHg), 98k of white dry crystals were obtai...
example 2
[0154] oxidized coenzyme Q 10 (100 g; purity 99.4%) was stirred and melted at 50°C. While stirring (power required for stirring: 0.3kw / m3), gradually add the prepared aqueous solution to the oily product, so that the reduction reaction is carried out at 50°C and a pH value of 4 to 6. The aqueous solution is the reducing agent Prepared by dissolving 100 g of sodium dithionite (purity: at least 75%) in 1000 ml of water. After two hours, the aqueous phase that contains oily product is removed from reaction mixture, then adds the ethanol that 1400g is heated to 50 ℃ in aqueous phase, stirs (stirring required power: 0.3kw / m 3 ), and the mixture was cooled to 2° C. to obtain a white crystalline slurry (flowable crystalline slurry is better). All the above operations were done under nitrogen atmosphere. The obtained crystalline slurry was filtered under reduced pressure, and the wet crystals were rinsed sequentially with cold water and cold ethanol (the temperature of the cold sol...
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