A kind of preparation method of 16a-hydroxyprednisolone
A technology of prednisolone hydroxyacetate and prednisolone hydroxyacetate, applied in chemical instruments and methods, steroids, organic chemistry, etc., can solve the problems of many impurities and low yield, and achieve simple and convenient production and operation, The effect of reducing the preparation cost and the production process is economical and environmentally friendly
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Embodiment 1
[0012] A. Preparation of solid-phase base catalyst
[0013] In a 1000ml three-necked flask, add a solution made of 50g of solid alumina, 300ml of tap water, 200ml of tap water and 15g of sodium carbonate, and stir the adsorption reaction at 25-30°C for 3-4 hours. After the reaction, evaporate the water under reduced pressure It was nearly dry, taken out and dried to obtain 50.1 g of solid-phase base catalyst with a water content of 5.6% and a weight yield of 102%.
[0014] B. Synthesis of 16a-hydroxyprednisolone
[0015] In a 2000ml three-necked flask, add 100g of the raw material 16a-prednisolone hydroxyacetate, 1500ml of toluene, and dissolve it completely under stirring, then add 30g of the above-mentioned solid-phase alkali catalyst, keep warm at 40-45°C and stir for hydrolysis reaction 6-8 Hours, TLC confirmed the reaction end point, after the reaction, while hot nitrogen pressure filtration, the filter cake was soaked and washed twice with 500ml toluene, and then the so...
Embodiment 2
[0017] A. Preparation of solid-phase base catalyst
[0018] According to the method described in A in the above-mentioned Example 1, only the alumina is replaced by silica gel, and 49.8 g of solid-phase alkali catalysts with silica gel as a carrier are obtained, and the water content is 6.8%.
[0019] B. Synthesis of 16a-hydroxyprednisolone
[0020] In a 2000ml three-neck flask, add 100g of raw material 16a-prednisolone hydroxyacetate, 1500ml of alcohol, stir to dissolve completely, then add 30g of solid-phase alkali catalyst, keep warm at 40-45°C and stir for 6-8 hours of hydrolysis reaction , TLC confirms the end point of the reaction, after the reaction is completed, filter under hot nitrogen pressure, soak and wash the filter cake twice with 500ml alcohol, then recover the solid-phase alkali catalyst and apply it mechanically; Lower the temperature, add tap water for water analysis, centrifuge, and decompress the filtrate to recover residual alcohol, then discharge it int...
Embodiment 3
[0022] A. Preparation of solid-phase base catalyst
[0023] According to the method described in A in above-mentioned embodiment one, just change aluminum oxide into calcium carbonate, sodium carbonate into sodium hydroxide, make the solid-phase base catalyst 49.6g with calcium carbonate as carrier, water content 4.8%.
[0024] B. Synthesis of 16a-hydroxyprednisolone
[0025] In a 2000ml three-necked bottle, add 100g of raw material 16a-prednisolone hydroxyacetate, 1500ml of chloroform, and dissolve it completely under stirring, then add 30g of the basic calcium carbonate solid-phase alkali catalyst prepared by the above-mentioned A, and keep it warm at 40 ~ Stir the hydrolysis reaction at 45°C for 6-8 hours, and confirm the end point of the reaction by TLC. After the reaction, press filter while hot nitrogen, soak the filter cake twice with 500ml chloroform, then recover the solid-phase alkali catalyst and apply it mechanically; the filtrate and the washing liquid are combine...
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