- Preparation method of amorolfine hydrochloride
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The invention relates to the technical field of pharmaceutical preparations. The invention discloses a preparation method of amorolfine hydrochloride. The method comprises the following steps: with 3-(4-tert-amylphenyl)-2-methyl propanol as a raw material, under alkaline condition, performing a reaction on the raw material with methylsulfonyl chloride and performing nucleophilic substitution reaction with cis-2,6-dimethylmorpholine; and finally performing a reaction with hydrogen chloride gas to form the amorolfine hydrochloride, that is, the final product. According to the present invention,the method has advantages of cheap raw material source, easily-controlled process operation, high yield, stable quality, less impurity, significantly-reduced cost compared to other methods, suitability for industrial production, and the like.
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Paragraph 0033; 0040-0043; 0050-0053; 0060-0062
(2020/10/05)
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- Preparation method of chiral morpholine compounds
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The invention discloses a preparation method of chiral morpholine compounds. The chiral morpholine compounds are prepared from alpha-methylcinnamic acid as a starting material by Friedel-Crafts reaction, amide bond construction reaction, reduction reaction and salinization reaction. The method has the following advantages: compared with the conventional technical route, tertiary amyl groups are introduced into the route in the method by Friedel-Crafts alkylation reaction, reaction yield is higher, and cost is lower; a condensing agent is used for construction of amide bonds, reaction conversion rate is high, and product purity is high; by catalytic hydrogenation based reduction of ethylenic bonds, reaction is clean, yield is high, and product purity is good; a metallic reducing agent is used for reducing carbonyl groups, use quantity of the reducing agent is small, conversion rate is high, and the method is applicable to large-scale industrial production.
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Paragraph 0004
(2019/02/03)
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- Amorolfine hydrochloride preparation method
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The invention provides an amorolfine hydrochloride preparation method which specifically comprises the following steps: putting a compound of formula IIa shown in the specification into an organic solvent, further putting an amidation catalyst, carrying out a stirring reaction, further adding cis-2,6-dimethyl morpholine, and carrying out a reaction so as to obtain a compound III; carrying out backflow stirring on the compound III in absolute methanol, adding magnesium chips in batches, and carrying out a reaction so as to obtain a compound IV; carrying out a reaction on the compound IV under the action of a reducing agent, thereby obtaining a compound V. The method is novel in process route, cheap and easy in raw material obtaining, low in cost, simple in process operation, short in production cycle, gentle in reaction condition, high in yield, good in product quality and applicable to industrial production.
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- PROCESS FOR THE PURIFICATION OF AMOROLFINE HYDROCHLORIDE
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The present invention relates to a process for the purification of amorolfine hydrochloride by means of a reversed-phase preparative high performances liquid chromatography (prep-HPLC) said method starting from a crude Amorolfine hydrochloride having purity higher than 90% and containing Bepromoline hydrochloride 5% and Fenpropimorf 3%. The process involves the use of a mobile phase comprising water and an organic solvent under isocratic conditions.
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- Process of producing amorolfine
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The present invention refers to an improved process of producing Amorolfine base, which is a compound of formula (I): said process comprising the steps of: (i) contacting a compound of formula (II): with a Friedel-Crafts catalyst; and (ii) adding one equivalent of 2-halogeno-2-methylbutane, characterised in that the reaction mixture obtained in step (i) is cooled to a temperature between -40 to -60 °C prior to step (ii) and the Friedel-Craft catalyst is chosen among the group consisting of boron trifluoride complex, titanium chloride complex, zinc chloride, gallium chloride, antimony pentafluoride, molybdenum pentachloride, indium chloride, antimony pentachloride, lanthanide bromide, scandium(III)triflate, lanthanide (III) triflate, yterbium (III) triflate and silica gel associated with ferric chloride.
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Page/Page column 11-12
(2008/12/06)
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- Process of producing bepromoline
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The present invention refers to a process of manufacturing a compound of formula (Ia): said process comprising: (i) contacting a compound of formula (III): with a compound of formula (IV): in the presence of a palladium catalyst, methanol and hydrogen gas
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Page/Page column 11-12
(2008/06/13)
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- INTERMEDIATE OF AMOROLFINE OR ITS SALT
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The present invention relates to a novel quaternary ammonium salt useful as a potential intermediate in the preparation of amorolfine and its salt. Further the invention also relates to the preparation of the intermediate.
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Page/Page column 6
(2008/06/13)
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- Process for producing 3-[4-(1,1-dimethyl-propyl)-phenyl]2-methyl-propionaldehyde and cis-4{3-[4-(1,1-dimethyl-propyl)-phenyl]2-methyl-propyl}-2,6-dimethyl-morpholine (amorolfine)
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The present invention discloses a new process for the preparation of 3-[4-(1,1-dimethyl-propyl)-phenyl]-2-methyl-propionaldehyde and for the preparation of cis-4-{3-[4-(1,1-dimethyl-propyl)-phenyl]-2-methyl-propyl}-2,6-dimethyl-morpholine (Amorolfine).
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Page/Page column 7
(2008/06/13)
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- PROCESS OF PRODUCING AMOROLFINE
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The present invention refers to an improved process of producing Amorolfine base, which is a compound of Formula (I) said process comprising the steps of: (i) contacting a compound of Formula (II) with a Friedel- Crafts catalyst at a temperature in the range of 20 to 30 °C; and (ii) adding one equivalent of 2-halogeno-2- methylbutane, characterised in that the reaction mixture obtained in step (i) is cooled to a temperature between -40 to -60 °C prior to step (ii).
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Page/Page column 13-16
(2008/06/13)
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