- Preparation method of prednisolone acetate
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The invention relates to prednisolone acetate and a preparation method of prednisolone acetate, which are characterized in that the prednisolone acetate is prepared by sequentially carrying out a biological fermentation, an esterification reaction, a bromination reaction and a debromination reaction on the raw material, the prednisolone acetate is subjected to a hydrolysis reaction to obtain prednisolone, the overall yield is up to 81.75%, and the HPLC area normalization content of prednisolone is up to 99.5%. The preparation method is short in synthetic route and low in cost, is suitable forindustrial production, and has a very high industrial value.
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- Preparation method of tetraene acetate
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The invention discloses a preparation method of tetraene acetate. The preparation method of tetraene acetate comprises a step of subjecting a compound 2 as described in the specification, a free radical type halogenating reagent, sulfur dioxide and an acid-binding agent to a reaction in an organic solvent so as to obtain a compound 1 as described in the specification, i.e., tetraene acetate. According to the preparation method, easily and commercially available prednisolone low in price is used as a starting raw material, hydroxyl groups of two different configurations are simultaneously eliminated in the one-step reaction, and intracyclic alkene is formed; and the method is reduced in reaction steps, mild in reaction conditions, simple in aftertreatment, high in yield, high in the chemical purity of a crude product and suitable for industrial production.
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Paragraph 0056-0065
(2019/12/25)
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- Optimization of the synthesis of a key intermediate for the preparation of glucocorticoids
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A short and efficient synthesis, based on a one-step double elimination, of a key intermediate in the synthesis of various glucocorticosteroids has been developed. This method can be carried out on large scale for further industrial applications. The synthesis allowed us to identify a novel prednisolone derivative 10 and its anti-inflammatory activity was determined in an in vivo model of inflammation. In order to understand the regioselectivity of the double elimination under various conditions, mechanistic studies were undertaken and confirmed the experimental results. We also propose a mechanism for the formation of the new steroid 10 studied by molecular modeling.
- Jouve, Romain,Thery, Vincent,Ducki, Sylvie,Helfenbein, Julie,Thiery, Jean-Christophe,Job, Aurélie,Picard, Elodie,Mallet, Christophe,Ripoche, Isabelle,Bennis, Khalil
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- C21 steroid 21 site acetylation process
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The invention discloses a C21 steroid 21 site acetylation process. C21 steroid is prednisolone, hydrocortisone, dexamethasone or betamethasone; the C21 steroid is subjected to acetylation with aceticanhydride; the acetylation of the C21 steroid with the acetic anhydride is carried out in a mixed solvent; an acetic acid alkali metal salt is adopted as a catalyst, and the reaction is carried out inthe presence of an inert gas; the mixed solvent is a mixed solvent of tetrahydrofuran and acetone; the weight ratio of the tetrahydrofuran to the acetone in the mixed solvent is (2-9):1. High-toxicity and high ammonia nitrogen pyridine and dimethylformamide are replaced by using the mixed solvent of tetrahydrofuran and acetone without ammonia nitrogen, no high ammonia nitrogen wastewater is generated, and environment pollution can be reduced.
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Paragraph 0010-0013
(2018/11/22)
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- Preparation process of prednisolone acetate
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The invention relates to a preparation process of prednisolone acetate. The preparation process comprises the steps that under the action of 4-dimethylamino-pyridine, no solvent needs to be additionally added, prednisolone and acetic anhydride directly react, the materials are flushed into water for separation, filtering and drying are carried out, and prednisolone acetate is prepared. The technical prejudice that in the prior art of the reaction process, pyridine or a pyridine-substituted solvent is generally used is overcome, the lot production capacity of a reaction still is greatly improved, and it is avoided that a large amount of industrial waste water hard to treat is generated. The process is simple in process, beneficial to environmental protection, low in cost and suitable for industrial large-scale production.
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Paragraph 0018; 0019; 0020
(2017/08/28)
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- A process for the preparation of prednisolone (by machine translation)
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The invention relates to a process for the preparation of prednisolone, including: to ACOH predinisone as raw materials, sequentially through the 3,20-keto-protection reaction and 11-keto-reduction reaction, 21-position hydroxy esterification reaction, 3,20- position alkone remove protection reaction, 21-bit b ester hydrolysis reaction is prednisolone. The present invention provides a first esterification, then deprotected of the new synthetic route, the deprotected process the nitrosation quenching reaction and resin hydrolysis reaction; an ester reaction in the mixed solvent and to complete the protection of inert gas, to avoid the hydrolysis reaction produces by-products. Process route of this invention is novel, the operation process is simple, the production cost is low, is suitable for industrial scale production. (by machine translation)
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Paragraph 0018; 0019
(2016/12/16)
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- Prednisolone acetate preparation method
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The present invention relates to a prednisolone acetate preparation method which is as follows: prednisolone acetate can be obtained by successive 3-site and 20-site keto-protection reaction, 11-site keto-reduction reaction, 21-site hydroxyl esterification reaction and 3-site and 20-site keto-deprotection reaction of prednisone acetate as a raw material. A new synthetic route of first esterification and then deprotection is provided, nitrosification quenching reaction and resin hydrolysis reaction can be omitted in the deprotection step, the technical process is greatly simplified, the cost of production is reduced, and the method is suitable for mass production.
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Paragraph 0027; 0028
(2016/10/17)
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- 9α-dehalogenation process
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The present invention involves improved processes for the dehalogenation of 9α-halosteroids (I) STR1 to produce the corresponding 11β-hydroxy steroids (II) STR2 which are known to be useful as pharmaceutical, where the improvements comprise (1) adding the 9α-halo steroid (I) to the chromium and (2) using catalytic amounts of chromium in the presence of a means of converting chromium (II) to chromium (III).
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- Process and intermediates for the preparation of 17 alphahydroxyprogesterones and corticoids from an enol steroid
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This invention discloses an improved process for the production of corticoids from 17α-hydroxy steroids utilizing peroxymonosulfate.
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