Technique for preparing 5'nucleotide bi-sodium
A technology for the preparation of disodium nucleotides, which is applied in the field of preparation of strong freshness aids, can solve the problems of cumbersome operation, impact on yield, poor 5'-position selectivity, etc., and reduce consumption and pollution , the effect of a simple post-processing process
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Embodiment 1
[0027] Add 50 grams of inosine, 500 grams of triethyl phosphate, and 3.4 grams of water into the reaction kettle, stir to cool down, add 87.5 grams of phosphorus oxychloride dropwise at about 5°C, and continue the reaction for 1.5 hours after dropping;
[0028] Cool down 900 grams of 10% sodium chloride solution to below 0°C, pour the above-mentioned reaction solution into it for hydrolysis while stirring, and then stand and separate for 20-60 minutes after 1 hour;
[0029] The hydrolyzed solution is naturally divided into triethyl phosphate and aqueous solution layer, the aqueous solution layer is cooled with 50% sodium hydroxide solution to adjust to PH ≥ 13, crystallized at 0 ℃ for 2-3 hours, and filtered;
[0030] The filtered solid is mainly sodium phosphate, the filtrate is neutralized with concentrated hydrochloric acid to PH=8-9, concentrated under reduced pressure to about 600 g remaining, cooled to 0-5°C, and filtered;
[0031] The filtered solid was crude disodium inosi...
Embodiment 2
[0033] 26.8 grams of inosine, 32.5 grams of guanosine, 650 grams of triethyl phosphate, and 3.6 grams of water were added to the reaction kettle, the temperature was lowered, 92 grams of phosphorus oxychloride was added dropwise at about 5°C, and the reaction was continued for 3 hours after dropping;
[0034] The temperature of 1000 grams of 10% sodium chloride solution is lowered to below 0°C, the above reaction liquid is poured into it for hydrolysis under stirring, and then it is allowed to stand for layering after 1 hour;
[0035] The hydrolyzed solution is naturally divided into a triethyl phosphate layer and an aqueous solution layer. The aqueous layer is cooled with 50% sodium hydroxide solution to adjust to PH≥13, crystallized at 0°C for 2-3 hours, and filtered;
[0036] The filtered solid is mainly sodium phosphate, the filtrate is neutralized with concentrated hydrochloric acid to PH=8-9, concentrated under reduced pressure to about 650 g remaining, cooled to 0-5°C, and ...
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