B01D9/005

LANTHANIDE COMPLEXES FOR CRYSTALLISING BIOLOGICAL MACROMOLECULES AND DETERMINING THE CRYSTALLOGRAPHIC STRUCTURE THEREOF

The invention relates to cationic complexes made up of a lanthanide ion Ln3+ and a ligand of formula (I) :

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with X, Y and R1 as defined in claim 1, and to the salts thereof with an anion, the solvates and hydrates thereof; with the exception of cationic complexes made up of a lanthanide ion Ln3+ and a ligand of one of formulae (I.1) or (I.4) as defined in claim 1, and the salts, solvates and hydrates thereof. The invention also relates to the use of such a complex or of a cationic complex made up of a lanthanide ion Ln3+ and a ligand of formula (I.1) or (I.4) as defined in claim 1, or of one of the salts thereof with an anion, the solvates or hydrates thereof, as an aid to the crystallisation of a biological macromolecule, as well as to crystallisation methods and methods for analysing or determining the structure of a biological macromolecule.

Process for the Preparation of Aclidinium Bromide

A process for preparing (3R)-3-[2-Hydroxy(di-2-thienyl)acetoxy]-1-(3-phenoxypropyl)-1-azoniabicyclo[2.2.2]octane bromide (aclidinium bromide) comprises reacting 2-hydroxy-2,2-dithien-2-ylacetic acid 1-azabicyclo[2.2.2]oct-3(R) yl methyl ester and 3-phenoxypropyl bromide, wherein the reaction takes place in a solvent or mixture of solvents selected from the group of amides and/or the group of solvents with a sulfoxide group. Also provided is a crystalline aclidinium bromide characterized by a powder XRPD pattern having peaks at 7.70.2 2, 10.40.2 2, 13.20.2 2, 13.80.2 2, 19.90.2 2, 20.30.2 2, 20.80.2 2, 24.20.2 2, 25.70.2 2, 26.10.2 2, 29.20.2 2, 30.80.2 2. A pharmaceutical composition comprises aclidinium bromide according to the invention and a pharmaceutically acceptable excipient.

SYNTHESIS OF TYROSINE DERIVED DIPHENOL MONOMERS
20180354892 · 2018-12-13 · ·

A method for preparing diphenol compounds includes adding a hydroxyphenyl carboxylic acid, a tyrosine ethyl ester, hydroxybenzotriazole hydrate and a solvent and stirring to produce a first solution. EDCl HCl is added to the first solution to produce a first mixture. Ethyl acetate is added to the first mixture to produce a second mixture. The second mixture is added to sodium chloride to produce a third mixture having layer separation. An aqueous layer is removed from the third mixture. The third mixture is extracted with reagents after the aqueous layer has been removed from the third mixture to produce a fourth mixture. Magnesium sulfate is added to the fourth mixture to produce a fifth mixture. The fifth mixture is filtered to produce filtrate. The filtrate is concentrated. Crystallization of the concentrated filtrate is induced. Methylene chloride is added to the crystallized filtrate to produce a solid product.

PROCESS FOR ISOLATING AND PURIFYING AMBROX
20180346434 · 2018-12-06 ·

A method of isolating and purifying ()-Ambrox from a reaction mixture comprising ()-Ambrox and one or more of the compounds (II), (III) and (IV)

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CRYSTALLIZATION OF 25-HYDROXY-7-DEHYDROCHOLESTEROL
20180327442 · 2018-11-15 ·

The present invention relates to a method of purification of compound of formula (I) which comprises the step of crystallization of compound of formula (I) from a composition comprising the compound of formula (I) and the compound of formula (II) and a specific solvent system containing ethanol, 1-propanol, 2-propanol, 2-methyl-1-propanol, 1-butanol or 2-butanol.

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Method for purifying mitomycin C

Provided are a method for purifying mitomycin C, comprising a step of recrystallizing crude mitomycin C crystals using a high-purity methanol; mitomycin C obtainable by the method; and the like.

CRYSTALLINE FORMS OF POSACONAZOLE INTERMEDIATE AND PROCESS FOR THE PREPARATION OF AMORPHOUS POSACONAZOLE

The present invention provides an industrial method production of amorphous posaconazole. The present invention also relates to a method for production of the posaconazole via and novel crystalline forms of posaconazole intermediate. More particularly the present invention relates to novel crystalline forms of posaconazole intermediate and methods for production of novel crystalline forms of posaconazole intermediate represented by the following structural formula III Which is key intermediate in the production of posaconazole. The present invention also provides for the one pot process for the preparation of amorphous posaconazole using novel crystalline forms of benzyl posaconazole.

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PROCESS FOR THE PREPARATION OF N-[4-[(3-CHLORO-4-FLUORO PHENYL) AMINO]-7-[[(3s-TETRAHYDRO-3-FURANYL]OXY]-6-QUINAZOLINYL]-4-(DIMETHYL AMINO)-(2E)-2-BUTENAMIDE (2Z)-2-BUTENEDIOATE (1 :2) AND ITS POLYMORPHS THEREOF

The present invention relates to an improved process for the preparation of N-[4-[(3-chloro-4-fluorophenyl)amino]-7-[[(3S)-tetrahydro-3-furanyl]oxy]-6-quinazolinyl]-4-(dimethyl amino)-(2E)-2-butenamide (2Z)-2-butenedioate (1:2) represented by the following structural formula:

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METHOD FOR SYNTHESIZING BIPYRIDINE COMPOUND AND METHOD FOR MANUFACTURING PYRIDINE COMPOUND

A target bipyridine compound is synthesized with high purity and a high yield in a simple and safe manner in a short period of time. A method for synthesizing a di-tert-butyl-2,2-bipyridine compound is provided, and the method includes a step of reacting, in a reaction solvent, a tert-butylpyridine compound with a dispersion product obtained by dispersing an alkali metal in a dispersion solvent. A method for synthesizing a bipyridine compound having no substituents is also provided, and the method includes a step of reacting, in a reaction solvent, pyridine with a dispersion product obtained by dispersing an alkali metal in a dispersion solvent.

POLYMORPHS OF 3-(4-AMINO-1-OXOISOINDOLIN-2-YL)PIPERIDINE-2,6-DIONE

The present application relates to polymorphs of Compound A:

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or a stereoisomer thereof, and methods of preparation and use thereof.