- Preparation method of halcinonide and derivative thereof
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The invention provides a preparation method of halcinonide and a derivative thereof. The method comprises the following steps: taking hydrocortisone acetate as a raw material, performing dehydration and then epoxidation on the raw material, performing ring opening, performing hydrolysis and chlorination, and then performing oxidation and ketalization, so as to obtain halcinonide; or performing dehydration and then epoxidation on the raw material, performing ring opening, performing hydrolysis, and then performing oxidation and ketalization, so as to obtain 9-fluoro-16a,17-(isopropylidenedioxy)corticosterone. In ring opening fluorination unit reaction, safe and mild reaction environment is selected, a fluorizating agent with low concentration is used as a reaction reagent, the reaction rate is effectively controlled, the production of side reaction products is restrained, and the product quality and yield are greatly improved. Moreover, in 16, 17-ketalization unit reaction, an acid catalyst which is low in toxicity and easy to control is adopted to replace boron trifluoride with high toxicity to perform catalysis, and the catalytic effect is effectively improved.
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- Preparation process of halcinonide intermediate
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The invention provides a prepration process of a halcinonide intermediate. The preparation process comprises the steps: taking a hydrofluoric acid-acetone mixed solvent as a solvent, slowly adding an intermediate N-3 at subzero 40 DEG C to subzero 30 DEG C, carrying out reaction for 4 to 8 hours after material feeding is completed, enabling the temperature to return to subzero 5 DEG C to 0 DEG C, continuously carrying out reaction for 10 to 30 min, slowly adding reaction fluid into a potassium carbonate solution after the reaction is completed, adjusting the PH value to 7.0 to 7.5, filtering and discharging a product, and drying the product to obtain the halcinonide intermediate with the structure as shown in formula N-5. According to the preparation process, a one-pot method is adopted for production, so that the production steps are effectively simplified, and the production period is shortened; the preparation process is more environment-friendly.
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Paragraph 0013
(2017/07/19)
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- Steroid esters
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The invention concerns compounds of formula I STR1 in which R1 is hydrogen or a straight or branched hydrocarbon chain; R2 is hydrogen or a straight or branched hydrocarbon chain; R3 is acyl; X1 is hydrogen, fluorine or chlorine; and X2 is hydrogen, fluorine or chlorine. Also disclosed are processes for preparation of the compounds, pharmaceutical compositions containing them and methods employing the compounds in the treatment of inflammatory and allergic conditions.
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- STEROID ESTERS
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Compounds of the general formula (I), in which formula the 1,2-position is saturated or is a double bond, R1 is hydrogen or a straight or branched hydrocarbon chain, R2 is hydrogen or a straight or branched hydrocarbon chain, R3 is acyl, X1 is hydrogen or halogen, X2 is hydrogen or halogen and provided that 1) R1 and R2 are not simultaneously hydrogen, 2) X1 and X2 are not simultaneously hydrogen, 3) when the 1,2-position is a double bond, R1 and R2 are not simultaneously methyl groups, 4) when the 1,2-position is a double, R1 is a hydrogen atom and R2 is a straight or branched hydrocarbon chain having 1-10 carbon atoms R3 is acyl having 11-20 carbon atoms, processes for their preparation, pharmaceutical preparations containing them and the use of the compounds in the treatment of inflammatory and allergic conditions
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