Crystallization process of 5'-nucleoside-sodium phosphate
A technology of sodium nucleoside monophosphate and nucleoside monophosphate, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as low yield and poor product quality, and achieve good repeatability, The effect of improving hygroscopicity and ensuring product quality
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Embodiment 1
[0025] Two parts of 5'-uridine monophosphate aqueous solution with a concentration of 100g / L, each 10L, were crystallized by conventional elution crystallization and the preparation method of this patent respectively. The former is directly adjusted to pH 7.5 with sodium hydroxide, and 10 L of ethanol is slowly added; the latter is adjusted to pH 6.0 with sodium hydroxide, and 30 g of sodium acetate and 10 L of ethanol are added. The two crystallization process conditions are the same, both controlled at 25° C., and the stirring speed is 50 rpm. After the crystallization was complete, the suspension was filtered with suction, washed with 85% ethanol, and dried in vacuo. Table 1 is a comparison of the product quality and crystallization yield of the two crystallization systems.
[0026] Table 1 Comparison of product quality and crystallization yield of two crystallization systems
[0027] project
Embodiment 2
[0029] Adjust 100L of 5'-uridine monophosphate aqueous solution with a concentration of 100g / L to pH 6.0 with sodium hydroxide, add 300g of sodium carbonate and 100L of methanol, and control the stirring speed at 25°C to 100rpm. After the crystallization was complete, the suspension was filtered with suction, and the resulting white crystals were washed with 85% ethanol and dried in vacuo to obtain 13.7 kg of 5'-uridine sodium crystals. The tested purity of the finished product is 98.3%, the water content is 19.8%, and the final crystallization yield is 95.1%. The test results are shown in Table 2.
[0030] Table 2 Quality inspection results of sodium uridine acid finished product: C 9 h 11 N 2 o 9 PNa 2 (molecular weight 368.15)
[0031] Test items
Embodiment 3
[0033] Adjust 100L of 5'-guanosine monophosphate aqueous solution with a concentration of 150g / L to pH 6.8 with sodium hydroxide, add 200g of sodium carbonate, control the stirring speed at 70rpm at 25°C, and add ethanol at a flow rate of 10L / h 120L. After the crystallization, the suspension was suction-filtered, the white crystals were washed with 85% ethanol, and dried in vacuo to obtain 18.2 kg of 5'-guanylic acid sodium salt crystals. The tested purity of the finished product is 99.7%, the water content is 11%, and the final crystallization yield is 95.5%. The test results are shown in Table 3.
[0034] Table 3 Quality inspection results of sodium guanylate finished product: C 10 h 12 N 5 o 8 PNa 2 (molecular weight 407.19)
[0035] Test items
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