Ethyl Corporation

Other

Albemarle Corporation

Aptuit (west Lafayette), LLC

S.s.c.i., Inc.

Aptuit (kansas City), LLC

Barbara C Stahly

G Patrick Stahly

Meng-Sheng Ao

Edward A Burt

Lester P Burton

Igor Ivanisevic

Donald R Hallenbeck

Simon Bates

Brigitte Benage

David E Bugay

Ronny W Lin

David Andrew Coates

Scott Lawrence Childs

Kenneth R Morris

E E Atkinson, Jr

Patricia M Mougin-Andres

The present disclosure relates to crystallizing a chemical substance(s) using ultrasound. Methods are provided for screening a chemical substance according to its solid forms by using ultrasound to generate new or unusual solid forms. Methods are also provided for crystallizing a chemical substance by novel techniques that include sonication. The present disclosure also relates to cocrystallization using ultrasound. Methods are provided for preparing cocrystals of an active agent and a guest by sonicating and crystallizing. Methods are also provided for screening a sample according to solid state phases (such as cocrystals and salts) and include generating a cocrystal from the sample using ultrasound.

Screening for solid forms by ultrasound crystallization and cocrystallization using ultrasound

A method of analyzing patterns. The method comprises: receiving a first diffraction pattern; receiving a second diffraction pattern; receiving a third diffraction pattern; determining a similarity between the first and second diffraction patterns; determining a similarity between the first and third diffraction pattern; determining a similarity between the second and third diffraction pattern; and performing hierarchical cluster analysis on the first and second diffraction pattern based on the determined similarity.

System and method for matching diffraction patterns

Methods for searching for possible forms of a sample and methods of screening a sample according to its form comprise disposing the sample in at least one receptacle that defines a capillary space, such as a capillary tube. The sample is solidified to generate at least one solid form or semisolid form, and the generated form is analyzed and classified. The analysis may determine differences in molecular arrangement of the various forms or characteristics that reflect the form. The methods may employ a plurality of samples, conditions, or receptacles in an effort to generate a variety of forms, so that all or a high percentage of possible forms are obtained.

Methods of screening for possible solid forms

The co-formation of diarylalkane by-product in the chloroalkylation of an aromatic compound with an ether corresponding to the formula R-O-R', wherein R is an .alpha.-chloroalkyl group containing at least two carbons and R' is R or alkyl, is minimized by conducting the reaction with agitation in the absence of a cosolvent and in the presence of both hydrogen sulfate and hydrogen chloride.

Chloroalkylation of aromatic compounds

The co-formation of diarylalkane by-product in the bromoalkylation of an aromatic compound with an ether corresponding to the formula R--O--R', wherein R is an .alpha.-chloroalkyl group containing at least two carbons and R' is R or alkyl, is minimized by conducting the reaction with agitation in the absence of a cosolvent and in the presence of both hydrogen sulfate and hydrogen bromide.

Bromoalkylation of aromatic compounds

Phosphorus compounds having at least one chlorine, bromine or iodine bonded directly to phosphorus are transhalogenated with fluorine by reaction with anhydrous hydrogen fluoride in an inert solvent, e.g., xylene, methylene chloride, in a manner such that said anhydrous hydrogen fluoride is added to said phosphorus compound at a rate such that said anhydrous hydrogen fluoride reacts with said phosphorus compound without the accumulation of an amount of unreacted anhydrous hydrogen fluoride which is sufficient to cause substantial decomposition of the desired fluorophosphorus product. A catalytic amount of a pyridine-type compound may optionally included in the reaction.

Process for transhalogenating a halophosphorus compound with fluoride

Phosphorus compounds having at least one chlorine, bromine or iodine bonded directly to phosphorus are transhalogenated with fluorine by reaction with anhydrous hydrogen fluoride in an inert solvent, e.g., xylene, methylene chloride, in a manner such that said anhydrous hydrogen fluoride is added to said phosphorus compound at a rate such that said anhydrous hydrogen fluoride reacts with said phosphorus compound without the accumulation of an amount of unreacted anhydrous hydrogen fluoride which is sufficient to cause substantial decomposition of the desired fluorophosphorus product.

Process for transhalogenating a halophosphorous compound with anhydrous

A monoalkylaromatic hydrocarbon is haloethylated to a 1-halo-1-arylethane with minimal co-formation of diarylalkane by-product by reacting it with hydrogen chloride or bromide and acetaldehyde in the presence of sulfuric acid only until not more than about 60% of the monoalkylaromatic hydrocarbon has been converted.

Haloethylation of aromatic hydrocarbons

1-Cyano-1-(4-alkylphenyl)alkenes having utility as chemical intermediates, especially in the preparation of ibuprofen and related pharmaceuticals, are prepared by reacting an alkylbenzene with an alkali metal cyanide and an acid halide in the presence of aluminum chloride.

Cyanoalkenylation process

A monoalkylaromatic hydrocarbon is haloethylated to a 1-halo-1-arylethane with minimal co-formation of diarylalkane and acetaldehyde by-products by reacting it with hydrogen chloride or bromide and a stoichiometric deficit of acetaldehyde in the presence of sulfuric acid in an amount such as to provide at least two mols of hydrogen sulfate per mol of acetaldehyde and less than 1.5 mols of hydrogen sulfate per mol of the monoalkylaromatic hydrocarbon.

A new process for preparing ibuprofen or its alkyl esters is provided. A 1-halo-1-(4-isobutylphenyl)ethane is reacted with carbon monoxide in the presence of water or an alcohol at a temperature between about 10.degree. C. and about 200.degree. C. An excess of several moles of water or alcohol is preferred. An acid such as hydrochloric acid may also be added. As catalyst, a palladium compound and at least one acid-stable ligand are present; however an excess of ligand over palladium is advantageous.

Process for preparing ibuprofen and its alkyl esters

Arylacetonitriles corresponding to the formula Ar-CH(R)CN are prepared by reducing a cyanohydrin corresponding to the formula Ar-C(R)(OH)CN with phosphorus pentasulfide in an inert solvent; Ar in the formulas representing aryl and R being hydrogen or alkyl. The products are primarily useful as pharmaceutical and agricultural intermediates.

Reduction of cyanohydrins

An amide is thiated to the corresponding thioamide by reacting it with phosphorus pentasulfide in the presence of an adjuvant selected from diatomaceous earth, zeolites, and molecular sieves.

Thiation process

Ammonium hydroxide is used in the recovery of a thiono compound prepared by reacting an organic carbonyl compound with phosphorus pentasulfide to improve the product yield.

Growing community of inventors

Baton Rouge, LA, United States of America

Barbara C Stahly