- Preparation method of glucocorticoid key intermediate
-
The invention provides a preparation method of a compound (III), which comprises the following steps: in an organic solvent, in the presence of a phase inversion catalyst and an organic acid, controlling the pH value of a reaction system to be 2-6, and oxidizing a compound (II) by potassium permanganate to obtain the compound (III). The invention also provides application of the preparation methodin preparation of budesonide.
- -
-
Paragraph 0060-0117
(2021/03/31)
-
- Method for preparing 16 alpha-hydroxyprednisolone
-
The invention discloses a method for preparing 16 alpha-hydroxyprednisolone, belonging to the technical field of medicine preparation and processing. According to the method, 21-hydroxypregna-1,4,9(11),16-tetraene-3,20-dione 21-acetate is used as an initial raw material and subjected to oxidation, bromo-hydroxylation, debromination and alcoholysis to prepare 16 alpha-hydroxyprednisolone. Accordingto the method for preparing 16 alpha-hydroxyprednisolone, generation of impurities in the reaction process can be effectively controlled by improving the defects of a traditional process, reaction process is mild, and an overall conversion rate is high; and the method disclosed by the invention has the advantages of low requirements on a reaction device, low operation cost, simplicity and convenience in operation, suitability for industrial production and higher market prospects.
- -
-
Paragraph 0011; 0030; 0033; 0035; 0038; 0040; 0043
(2020/07/02)
-
- A budesonide industrial preparation method (by machine translation)
-
The invention relates to a cloth budesonide industrial preparation method. Specifically, the invention relates to a hydrochloric acid aqueous solution, dichloromethane and in acetonitrile, 16 α - hydroxy prednisolone with butyraldehyde by the reaction of the budesonide. In the method of the present invention has the industrial can be implemented on, repeatability and the like. (by machine translation)
- -
-
Paragraph 0039; 0044-0045
(2019/03/10)
-
- Preparation method of 16a-hydroxy prednisolone acetate product
-
A preparation method of a 16a-hydroxy prednisolone acetate product includes dissolving 17-dehydroxy prednisone acetate as a raw material in an organic solvent, oxidizing 16 and 17 double bonds by potassium permanganate under acid catalysis to obtain an oxide, dissolving the obtained oxide in an organic solvent, adding acetone, and carrying out acid catalyzed reaction to obtain a protector; dissolving the protector in an organic solvent, adding a reducing agent to reduce ketone at the 11th position, directly adding an acid water solution for hydrolysis and deprotection after the reduction reaction to obtain 16a-hydroxy prednisolone acetate, and subjecting the crude product to decoloration and recrystallization by low-carbon-alcohol heating reflux to obtain the 16a-hydroxy prednisolone acetate product. Although two reaction steps, protection and deprotection, are added, the reaction yield of units in each step is high, the method is simple and convenient to operate, the process is economical and environmentally friendly, and the total synthesis yield is increased remarkably; the preparation cost of the preparation method is 20-25% lower than that of conventional production methods.
- -
-
Paragraph 0031; 0038-0041; 0048-0049; 0051; 0058-0059
(2019/05/22)
-
- Preparation method of 16a-prednisolone hydroxyacetate
-
Disclosed is a preparation method of 16a-prednisolone hydroxyacetate. The method comprises dissolving 17-prednison dehydroxylated acetate as the raw material into organic solvent, under catalysis of acids, oxidizing 16th and 17th double bonds through potassium permanganate to obtain an oxide, and dissolving the oxide into acetone for acid-catalyzed reaction to obtain a protector; dissolving the protector into organic solvent, adding in reducing agent to reduce 11th ketone, then directly adding in acid aqueous solution for hydrolysis and deprotection to obtain the 16a-prednisolone hydroxyacetate. Although the preparation method of the 16a-prednisolone hydroxyacetate adds the two reaction steps of protection and deprotection, every unit reaction is high in yield, the third and fourth reaction steps can be completed within on pot, so that the production operation can be simple and convenient, the production processes are economical and environmentally friendly, the problems of many side reactions and impurities and difficulty impurity refining of oxidation reaction in traditional production process can be greatly solved, the total synthesizing yield can be greatly increased, and compared with traditional production methods, the preparation method of the 16a-prednisolone hydroxyacetate can reduce the production cost by 20-25%.
- -
-
Paragraph 0036; 0037; 0046; 0047; 0056; 0057
(2019/04/17)
-
- NOVEL PROCESS FOR PREPARATION OF GLUCOCORTICOID STEROIDS
-
The present invention discloses a process for the preparation of 16, 17-acetals of pregnane derivatives having formula (I) wherein each substituent is independently selected from; R1 is H or CH3; R2 is C1-C6 linear or branched alkyl, alkynyl group or cycloalkyl group; aryl or heteroaryl group; or R1 and R2 combine to form saturated, unsaturated C3-C6 cyclic or heterocyclic ring; R3 and R4 are same or different and each independently represents H or halogen; R5 is -OH or –OCOR wherein R represents H or C1-C6 linear, branched or cyclic alkyl group that may be substituted.
- -
-
Page/Page column 13; 14
(2016/08/23)
-
- A kind of budesonide S isomer R isomer method of preparation
-
The invention discloses a method for preparing an R-isomer by using an S-isomer of budesonide. The method comprises the steps: enabling budesonide and acetic anhydride to be subjected to esterification reaction to obtain budesonide acetate; then, carrying out oxidative ring cleavage under the action of a strong oxidant to obtain 16-alpha hydroxyprednisonlone acetate; and condensing butyraldehyde and the 16-alpha hydroxyprednisonlone acetate to obtain budesonide acetate, and hydrolyzing to obtain R-budesonide. The method disclosed by the invention is high in conversion rate, high in yield and capable of effectively converting the S-isomer of the budesonide into the R-isomer.
- -
-
Paragraph 0008; 0020-0021
(2017/01/12)
-
- One-pot processes for preparing prednisolone derivatives
-
Disclosed is a one-pot process for the preparation of a prednisolone derivative of formula I, comprising reacting the compound of formula II with the compound of formula III and the compound of formula IV The process does not need to separate and purify t
- -
-
Page/Page column 4
(2008/06/13)
-
- 9α-dehalogenation process
-
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).
- -
-
-