- Preparation method of
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The invention provides a preparation method of and an intermediate thereof. The preparation method comprises the following steps: carrying out chlorination reaction on the compound of the formula N - 7 N - 3 with a chlorination reagent, then carrying out a fluorine reaction with the fluorine-containing reagent, and reacting the compound as follows. Of these, the chlorinating agent is selected from the sulfonyl chlorides of aromatic hydrocarbons, in particular benzenesulfonyl chloride. At least one of p-toluenesulfonyl chloride and p-chlorobenzoyl chloride, wherein the fluorine-containing agent is hydrofluoric acid. The preparation method is efficient, green and environment-friendly, shortens the production cycle, reduces a large amount of wastewater, improves the yield, reduces the production cost, realizes clean production, HPLC content of the product is less than 99.0%, and the yield reaches 0.10% 100% or more.
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- Synthesis method and application of 9-fluorosteroid compound
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The invention provides a synthesis method and application of a 9-fluorosteroid compound, and relates to the technical field of chemical synthesis. The synthesis method of the 9-fluorosteroid compoundcomprises the following step: reacting a compound II in an ionic liquid containing hydrogen fluoride salt to obtain a 9-fluorosteroid compound III. According to the synthesis method of the 9-fluorosteroid compound, the ionic liquid containing the hydrogen fluoride salt is used as a fluorinating agent to replace a traditional hydrogen fluoride aqueous solution, volatilization of hydrogen fluoride gas is avoided, corrosivity is small, toxicity is greatly reduced, reaction conditions are mild, reaction can be completed at the room temperature, operability is high, the safety coefficient is high,and production applicability is improved. The synthesis method of the 9-fluorosteroid compound is used for preparing corticosteroid drugs, highly toxic chemical reagents are not used in the synthesisroute, the operability is high, the safety coefficient is high, and the production applicability is improved.
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Paragraph 0089-0096; 0111-0114
(2021/01/15)
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- Preparation method of halcinonide
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The invention provides a preparation method of halcinonide. The method includes: (1) chlorination reaction: in the presence of SO2, reacting a compound 1 with a chlorination reagent to generate a compound 2, with the chlorination reagent being selected from one or more of acetyl chloride, propionyl chloride, benzoyl chloride, lithium chloride, carbon tetrachloride, chlorosuccinimide and dichloro dimethylhydantoin; and (2) ring-opening reaction: reacting the compound 2 with hydrogen fluoride to obtain halcinonide. The method provided by the invention has the beneficial effects of mild reactionconditions, friendly environment, easy operation and low cost, has industrialization value, can effectively control side reaction, and improve the reaction yield and quality; the process design does not involve high-risk reaction, and is easy to realize industrialization; high-pollution reaction does not exist, thus easing the pressure of environmental protection treatment.
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Paragraph 0006; 0043-0049
(2019/01/24)
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- Steroid 21-hydroxyl chlorination or bromination method
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The invention discloses a steroid 21-hydroxyl chlorination or bromination method. A compound shown as formula A is adopted as the start material, and in the presence of SO2, reaction with a chlorination or bromination reagent is carried out to prepare a compound shown as formula B. The method provided by the invention has the characteristics of mild process conditions, environmental friendliness,easily available reagents, easy operation, low cost and high yield, and is suitable for industrial mass production.
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Paragraph 0057-0059
(2019/01/24)
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- Pregnane derivatives 16, 17 - acetal (ketone) preparation method
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Disclosed is a method for preparing a pregnane derivative 16,17-acetal (ketal) compound shown in the general formula I, the method comprising the step of reacting a compound of a general formula II with a compound of a general formula III or a general formula IV in the presence of boron trifluoride, wherein the dotted line between site 1 and site 2 denotes a saturated or unsaturated bond; R is hydroxyl, halogen or -OCOR7, wherein R7 is a C1-C12 linear chain or branched alkyl, a C3-C10 cycloalkyl, a C2-C8 alkenyl or a C2-C8 alkynyl; R1 and R2 are each hydrogen, a C1-C12 linear chain or branched alkyl, a C3-C10 cycloalkyl, a C2-C8 alkenyl or a C2-C8 alkynyl, or R1, R2 and the carbon to which they are connected form a C3-C10 cycloalkyl together, with the provision that R1 and R2 are not hydrogen simultaneously; R3 is hydrogen or -OCOR8, wherein R8 is a C1-C12 linear chain or branched alkyl, or a C3-C10 cycloalkyl; R4 is hydrogen, fluorine or chlorine; R5 is hydrogen, fluorine, chlorine or methyl; and R6 is a C1-C12 linear chain or branched alkyl. Compared with current processes, the method causes little pollution to the environment, has relatively mild reaction conditions, ease of control, reduced energy consumption and low production costs.
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Paragraph 0046-0048
(2017/08/31)
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- Method for reducing or preventing transplant rejection in the eye and intraocular implants for use therefor
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Methods for reducing or preventing transplant rejection in the eye of an individual are described, comprising: a) performing an ocular transplant procedure; and b) implanting in the eye a bioerodible drug delivery system comprising an immunosuppressive agent and a bioerodible polymer.
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- Composition for the topical treatment of poison ivy and other forms of contact dermatitis
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Composition for topical administration comprising (a) a corticosteroid, and (b) a drying agent.
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- Mucosal adhesive device for long-acting delivery of pharmaceutical combinations in oral cavity
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Mucosal adhesive devices are provided for use in the oral cavity for therapy against infections. The devices are dosage units which comprise a combination of antimicrobial agents such as antifungal agents and anti-inflammatory agents, optionally also a local anesthetic. The dosage units yield a gradual and relatively constant release of the pharmaceuticals over at least a 12-hour period.
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- A New Method of Transforming 11β,17α,21-Trihydroxy-20-oxo Steroids into the 21-Chloro-20-oxo-Δ9(11),16 Derivatives
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Reaction of the 17α nitrates 1a,b with lithium chloride in hexamethylphosphoric triamide or N-methylpyrrolidone results in formation of the Δ16 steroids 2a,b by elimination of the 17α nitrooxy group.The corresponding 21 mesylates 1c,d are transformed into the 21-chloro-Δ16 steroids 2b,c under the same conditions.When the reaction was carried out with the 11β,17α-dinitrooxy-21-mesyloxy derivatives 4, the 21-chloro-Δ9(11),16 steroids 5 were obtained. 5a is a suitable intermediate for a short synthesis of 10, a topical anti-inflammatory corticosteroid.
- Annen, Klaus,Hofmeister, Helmut,Laurent, Henry,Wiechert, Rudolf
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p. 966 - 972
(2007/10/02)
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