Preparation method of 5alpha, 6alpha-epoxy-11beta, 17alpha-dihydroxypregna-3, 20-diethylene glycol ketal
A technology of diethylene glycol ketal and hydroxypregna, which is applied in the field of biocatalysis to achieve the effect of avoiding risks and avoiding adverse effects
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Embodiment 1
[0022] (1) Catalyst screening: screening commercially available immobilized lipase NOV 40086, biodiesel NS81006, Vland lipase enzyme solution TG, TM, R, LIP O, immobilized lipase numbered 0428, 0415, Vland 8340, immobilized Lipase IM and lipase LIP F, respectively, catalyze the epoxy reaction.
[0023] (2) Biotransformation process: Catalytic epoxy reaction system contains 50mM substrate 6-methyl reductant, 1M acetic acid / sodium acetate buffer (pH 5.8), ethyl acetate 7.5% (v / v), substrate: octanoic acid : Hydrogen peroxide is 1:5:8, hydrogen peroxide (30% H 2 o 2 Aqueous solution) is added once, and then add different catalysts (compared to the mass percentage of the substrate, w / w, the enzyme solution is based on the system volume ratio, and the immobilized enzyme or enzyme powder is based on mass), and the reaction is started at 30°C and 220rpm .
[0024] (3) Liquid phase detection process: After the conversion is completed, the yield or purity is detected by liquid phase...
Embodiment 2
[0032] 1M acetic acid / sodium acetate buffer (pH 5.8) contains 200g / L substrate 6-methyl reduction, ethyl acetate 7.5% (v / v), substrate: caprylic acid: hydrogen peroxide ratio 1:5:8, Hydrogen peroxide (30% H 2 o 2 After one addition of aqueous solution), 65% (w / w) of immobilized lipase LIP F was added to the reaction system and reacted at different reaction temperatures. After the reaction, the liquid phase detection method in Example 1 was used to measure the yield, and the results are shown in Table 2, preferably 30° C. is the optimum reaction temperature.
[0033] Comparison of different reaction temperatures in table 2
[0034]
Embodiment 3
[0036] In order to reduce the cost, enzyme powder was used instead of immobilized lipase LIP F, and the appropriate amount of catalyst was optimized. The optimized system is 1M acetic acid / sodium acetate buffer solution (pH 5.8) containing 200g / L substrate 6-methyl reducer, ethyl acetate 7.5% (v / v), substrate: octanoic acid: hydrogen peroxide at 1:5 : 8, hydrogen peroxide (30% H 2 o 2 After one addition of aqueous solution), LIP F enzyme powder of different quality was added to the reaction system, and the reaction was started at 30°C and 220rpm. After the reaction finishes, adopt the liquid phase detection method in the embodiment 1 to survey the product purity in the reaction solution, the result is as shown in table 3, considering cost and impurity content comprehensively, the LIP F enzyme powder addition of preferred 7.5% (w / w) , and the yield was 75.62%.
[0037] The influence of table 3 catalyst dosage on epoxy reaction
[0038]
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