221615-75-4Relevant articles and documents
Etoricoxib purification and preparation method
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Paragraph 0065; 0136-0138; 0145-0147; 0152-0154; 0159-0161, (2019/04/17)
The invention relates to an etoricoxib purification method which includes the operation: performing reduction reaction on etoricoxib crude drugs to be purified and reduction agents in solvents. The invention further relates to a method for preparing etoricoxib. The purity of the finished etoricoxib prepared by the preparation method is higher than 99.9%, the total content of an impurity F, an impurity 20 and an impurity 21 is lower than 0.001%, and no impurity M is detected.
Continuous flow production process for etoricoxib intermediate
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Paragraph 0036; 0044; 0051-0054; 0062-0065, (2018/11/04)
The invention discloses a continuous flow production process for an etoricoxib intermediate, belonging to the field of application technologies for bulk pharmaceutical chemical production in fine chemical engineering processes. The method for the etoricoxib intermediate comprises the following steps: step 1, synthesis of an intermediate in a continuous flow microreactor with non-nucleophilic organic strong base as a reagent; and step 2, performing of an oxidation process in the continuous flow microreactor by using a cheap inorganic oxidant under the action of a transition metal catalyst. Themethod comprises the following concrete reaction steps: with 4-(methylthio)phenylacetic acid and methyl 6-methylpyridine-3-carboxylate as starting materials, allowing the 4-(methylthio)phenylacetic acid and the methyl 6-methylpyridine-3-carboxylate to undergo a two-step reaction in the continuous flow microreactor so as to form 1-(6-methylpyridin-3-yl)-2-(4-methylsulfonylphenyl)ethanone. The method provided by the invention adopts novel reagents and catalyst and innovative equipment, has a yield of more than 70%, well controls generation of reaction heat and gas, and has the characteristics ofnovel catalysts, relatively mild reaction conditions, etc.
Method for preparing etoricoxib
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Paragraph 0046; 0047; 0048, (2017/08/02)
The invention discloses a method for preparing etoricoxib, and provides a method for preparing etoricoxib I. The method comprises the following step: performing neutralization reaction on hydrohaloride of the etoricoxib I and alkali in a halogenated hydrocarbon solvent to obtain the etoricoxib I, wherein X is halogen. The preparation method is mild in reaction condition, simple and safe in operation and high in yield, no special purification equipment is required, column chromatography separation operation in a posttreatment process is avoided, and the prepared etoricoxib is high in purity (the purity is equal to or higher than 99.5 percent, the content of all impurities is equal to or lower than 0.10 percent, and a raw medicament standard can be met), low in cost and suitable for industrial production.
Preparation of relying on tests the past intermediate 1 - (6 - methyl pyridine - 3 - yl) - 2 - [4 - (methylsulfonyl) phenyl] ethanone method
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, (2017/08/25)
The invention provides a preparation method of 1-(6-methylpyridyl-3-yl)-2-[4-(mesyl)-phenyl]-ethyl-one, which is characterized by comprising the following steps: (1) adding a compound B and an organic metal reagent into (4-dimethylsulfido)phenylacetic acid or metal salt (A) thereof to perform condensation reaction to obtain a compound C disclosed in the specification, wherein M is selected from H or metals and is preferably H or an alkali metal, and R is selected from H or C1-C6 alkyl groups; and (2) oxidizing the compound C with oxydol to obtain a compound D disclosed in the specification. In the two-step synthesis process, the yield from the compound A to the compound C is about 85%, the yield from the compound C to the compound D is about 90%, and the total mole yield is 65-80%; and the HPLC (high performance liquid chromatography) purity of the compound D is higher than 98%.Compared with the prior art, the method provided by the invention has the advantages of higher product quality and lower cost.
The Process For Preparing a Ketosulfone Derivative
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Paragraph 0068; 0069, (2015/05/26)
The present invention relates to a process for preparing a ketosulfone derivative and, more particularly, to an improved method for synthesising 1-(6-methylpyridin-3-yl)-2-[(4-methylsulfonyl)-phenyl]ethanone by means of Pd-catalysed alpha arylation process of a heteroaromatic ketone derivative.
Very efficient process for preparing an intermediate of Etoricoxib
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Paragraph 0048-0052, (2014/08/06)
The present invention relates to an efficient process for preparing 1-(6-methylpyridin-3-yl)-2-[4-(methylsulfonyl)phenyl]ethanone, an intermediate of the synthesis of Etoricoxib. Water is employed as reaction medium.
Very efficient process for preparing an intermediate of etoricoxib
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Page/Page column, (2014/07/08)
The present invention relates to an efficient process for preparing 1-(6-methylpyridin-3-yl)-2-[4-(methylsulfonyl)phenyl]ethanone, an intermediate of the synthesis of Etoricoxib. Water is employed as reaction medium.
Novel process for the preparation of 1-(6-methylpyridin-3-yl)-2-[4-(methylsulfonyl)phenyl]ethanone, an intermediate of etoricoxib.
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, (2013/03/26)
The present invention refers to a novel process for the preparation of 1-(6-methylpyridin-3-yl)-2-[4-(methylsulfonyl)phenyl]ethanone, an intermediate of the synthesis of Etoricoxib, an active ingredient on which the Arcoxia drug is based.
PROCESS FOR CYCLOOXYGENASE-2 SELECTIVE INHIBITOR
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, (2013/09/26)
The present invention describes a process for preparing a cyclooxygenase-2 selective inhibitor. It provides a synthetic procedure for the said substance namely 5-chloro-3-(4-methylsulphonyl)phenyl-2-(2-methyl-5-pyridinyl)pyridine of formula (I). The invention also relates to preparation of a new intermediate of formula (IV) and a process to prepare it. Furthermore, the invention describes a process for preparing another key intermediate of formula (II). Compounds of formula (IV) and formula (II) are useful intermediates in synthesis of the said cyclooxygenase-2 inhibitor.
A convenient synthesis of the key intermediate of selective COX-2 inhibitor Etoricoxib
Tartaggia, Stefano,Caporale, Andrea,Fontana, Francesco,Stabile, Paolo,Castellin, Andrea,De Lucchi, Ottorino
, p. 18544 - 18549 (2013/10/21)
An original strategy for the synthesis of ketone 1, the key intermediate for preparing Etoricoxib, an important nonsteroidal anti-inflammatory drug, has been developed. Inexpensive 5-hydroxy-2-methylpyridine was converted to the corresponding acetyl derivative in four practical synthetic steps. The following palladium-catalyzed α-arylation of acetylpicoline with 4-bromo- or 4-chlorophenyl methyl sulfone was efficiently optimized in order to afford ketone 1 in remarkable yield.
