Preparation process of 3-deacetylated-7-amino-cephalosporanic acid
A technology for aminocephalosporanic acid and deacetylation, which is applied in the field of medicine, can solve the problems of low yield, long process route, and many product losses, and achieves the effects of high product yield and short process route.
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Embodiment 1
[0033] a. Weigh 4.1KU cephalosporin acylase and 2.2KU cephalosporin esterase respectively, wash them with anhydrous brine, and put them into a 2.0L enzyme reactor;
[0034] b. Take the cephalosporin C nanofiltration concentrated solution analyzed by sodium bicarbonate with a concentration of 45.6g / L and prepare 1.2L of cephalosporin C solution with a concentration of 30.2g / L and put it into a 2.0L enzyme reactor , the stirring speed is 400rpm, the pH is controlled by 3mol / L ammonia water to be 8.05, the temperature is 18°C, and after 80 minutes of reaction, the reaction solution is transferred to a 2L beaker (cephalosporin acylase and cephalosporin esterase are absorbed by the bottom of the enzyme reactor. sieve retention);
[0035] c. Cool the reaction solution to 5°C, add 10% hydrochloric acid dropwise to adjust the pH to 5.85, let it grow for 30 minutes, then continue to add hydrochloric acid to pH 4.01, grow the crystal for 4 hours, filter with suction, wash twice with 1...
Embodiment 2
[0037] a. Weigh 7.5KU cephalosporin acylase and 3.1KU cephalosporin esterase respectively, wash them with anhydrous brine, and put them into a 2.0L enzyme reactor;
[0038] b. Take the cephalosporin C nanofiltration concentrate that is analyzed by sodium acetate with a concentration of 56.7g / L and prepare 1.2L of cephalosporin C solution with a concentration of 36.8g / L with no salt water, and put it into a 2.0L enzyme reactor. The stirring speed is 400rpm, the pH is controlled to be 8.10 with 3mol / L ammonia water, and the temperature is 20°C. After reacting for 90min, the reaction solution is transferred to a 2L beaker (cephalosporin acylase and cephalosporin esterase are sieved by the bottom of the enzyme reactor. net intercept);
[0039] c. Cool the reaction solution to 5°C, add 10% hydrochloric acid dropwise to adjust the pH to 5.80, let it grow for 30 minutes, then continue to add hydrochloric acid dropwise to pH 4.08, grow the crystal for 4 hours, filter with suction, was...
Embodiment 3
[0041] a. Weigh 10KU cephalosporin acylase and 4.0KU cephalosporin esterase respectively, wash them with anhydrous brine, and put them into a 2.0L enzyme reactor;
[0042]b. Take the cephalosporin C nanofiltration concentrate that is analyzed by sodium acetate with a concentration of 56.7g / L and prepare 1.2L of cephalosporin C solution with a concentration of 44.6g / L with no salt water, and put it into a 2.0L enzyme reactor. The stirring speed is 400rpm, the pH is controlled to be 8.30 with 3mol / L ammonia water, and the temperature is 20°C. After reacting for 90min, the reaction solution is transferred to a 2L beaker (cephalosporin acylase and cephalosporin esterase are sieved by the bottom of the enzyme reactor. net interception);
[0043] c. Cool the reaction solution to 5°C, add 10% hydrochloric acid dropwise to adjust the pH to 6.10, let stand to grow the crystal for 30 minutes, then continue to drop hydrochloric acid to pH 4.04, grow the crystal for 4 hours, filter with ...
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