C07C253/34

METHOD FOR PRODUCING PURIFIED PHTHALONITRILE AND METHOD FOR PURIFYING PHTHALONITRILE

A method for producing a purified phthalonitrile is described. The method involves reacting ammonia, oxygen, and xylene in the presence of a catalyst to obtain a product gas containing a phthalonitrile and a cyanobenzamide and then contacting the reaction product gas with an organic solvent to obtain a collection liquid. The collection liquid is distilled by a high boiling point fraction-separating column to obtain a gas that contains the phthalonitrile and the organic solvent from the column top, and to obtain a bottom liquid that contains a cyanobenzamide from the column bottom. The bottom liquid has a phthalonitrile content of 90% by mass or less. The bottom liquid is subjected to combustion, while being kept in a liquid state, and the purified phthalonitrile is obtained by removing the organic solvent from the gas that has been obtained from the column top.

METHOD FOR PRODUCING PURIFIED PHTHALONITRILE AND METHOD FOR PURIFYING PHTHALONITRILE

A method for producing a purified phthalonitrile is described. The method involves reacting ammonia, oxygen, and xylene in the presence of a catalyst to obtain a product gas containing a phthalonitrile and a cyanobenzamide and then contacting the reaction product gas with an organic solvent to obtain a collection liquid. The collection liquid is distilled by a high boiling point fraction-separating column to obtain a gas that contains the phthalonitrile and the organic solvent from the column top, and to obtain a bottom liquid that contains a cyanobenzamide from the column bottom. The bottom liquid has a phthalonitrile content of 90% by mass or less. The bottom liquid is subjected to combustion, while being kept in a liquid state, and the purified phthalonitrile is obtained by removing the organic solvent from the gas that has been obtained from the column top.

PROCESSES OF MAKING 3-FLUORO-5-(((1S,2aR)-1,3,3,4,4-PENTAFLUORO-2a-HYDROXY-2,2a,3,4-TETRAHYDRO-1H-CYCLOPENTA[CD]INDEN-7-YL)OXY)-BENZONITRILE AND POLYMORPHS THEREOF
20230115881 · 2023-04-13 ·

The present disclosure provides certain processes of making 3-fluoro-5-(((1S,2aR)-1,3,3,4,4-pentafluoro-2a-hydroxy-2,2a,3,4-tetrahydro-1H-cyclopenta[cd]inden-7-yl)oxy)-benzonitrile (Compound 1) and certain polymorphs thereof. Also provided are pharmaceutical compositions comprising a crystalline polymorph form of Compound 1 and processes for preparing such polymorph forms.

PROCESSES OF MAKING 3-FLUORO-5-(((1S,2aR)-1,3,3,4,4-PENTAFLUORO-2a-HYDROXY-2,2a,3,4-TETRAHYDRO-1H-CYCLOPENTA[CD]INDEN-7-YL)OXY)-BENZONITRILE AND POLYMORPHS THEREOF
20230115881 · 2023-04-13 ·

The present disclosure provides certain processes of making 3-fluoro-5-(((1S,2aR)-1,3,3,4,4-pentafluoro-2a-hydroxy-2,2a,3,4-tetrahydro-1H-cyclopenta[cd]inden-7-yl)oxy)-benzonitrile (Compound 1) and certain polymorphs thereof. Also provided are pharmaceutical compositions comprising a crystalline polymorph form of Compound 1 and processes for preparing such polymorph forms.

ACETONITRILE PURIFICATION PROCESS FOR ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETER
20230073691 · 2023-03-09 ·

The present invention relates to the technical field of acetonitrile refining, and in particular, to an improved acetonitrile purification process for an ultrahigh performance liquid chromatography-mass spectrometer. The present invention provides an acetonitrile purification process. A high-purity finished product may be obtained by performing operations of oxidation, rectification adsorption, drying, reflux rectification and filtration on industrial acetonitrile and controlling related parameters such as temperature, flow and the like, continuous production is ensured, a light transmittance of the finished product in ultraviolet rays of 200 to 260 nm is greater than or equal to 95%, water and impurities in the industrial acetonitrile are removed, and the requirements of the ultrahigh performance liquid chromatography-mass spectrometer are met; moreover, by controlling process parameters and equipment.

ACETONITRILE PURIFICATION PROCESS FOR ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETER
20230073691 · 2023-03-09 ·

The present invention relates to the technical field of acetonitrile refining, and in particular, to an improved acetonitrile purification process for an ultrahigh performance liquid chromatography-mass spectrometer. The present invention provides an acetonitrile purification process. A high-purity finished product may be obtained by performing operations of oxidation, rectification adsorption, drying, reflux rectification and filtration on industrial acetonitrile and controlling related parameters such as temperature, flow and the like, continuous production is ensured, a light transmittance of the finished product in ultraviolet rays of 200 to 260 nm is greater than or equal to 95%, water and impurities in the industrial acetonitrile are removed, and the requirements of the ultrahigh performance liquid chromatography-mass spectrometer are met; moreover, by controlling process parameters and equipment.

ACETONITRILE PURIFICATION PROCESS FOR ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETER
20230073691 · 2023-03-09 ·

The present invention relates to the technical field of acetonitrile refining, and in particular, to an improved acetonitrile purification process for an ultrahigh performance liquid chromatography-mass spectrometer. The present invention provides an acetonitrile purification process. A high-purity finished product may be obtained by performing operations of oxidation, rectification adsorption, drying, reflux rectification and filtration on industrial acetonitrile and controlling related parameters such as temperature, flow and the like, continuous production is ensured, a light transmittance of the finished product in ultraviolet rays of 200 to 260 nm is greater than or equal to 95%, water and impurities in the industrial acetonitrile are removed, and the requirements of the ultrahigh performance liquid chromatography-mass spectrometer are met; moreover, by controlling process parameters and equipment.

High purity 2-naphthylacetonitrile and method for producing same

High purity 2-naphthylacetonitrile with fewer impurities can be used as a starting material or intermediate for synthesizing various pharmaceutical products, agricultural chemicals, and chemical products, and a production method thereof. A high purity 2-naphthylacetonitrile having an HPLC purity of 2-naphthylacetonitrile of not less than 95 area %, and containing naphthalene compounds represented by the formulas (a)-(j) at a content of a predetermined area % or below. A method for producing high purity 2-naphthylacetonitrile, may include: subjecting 2′-acetonaphthone to a Willgerodt reaction in the presence of an additive where necessary, and hydrolyzing the obtained amide compound to give 2-naphthylacetic acid; and reacting the 2-naphthylacetic acid obtained in the subjecting, a halogenating agent and sulfamide in the presence of a catalyst as necessary in an organic solvent to give 2-naphthylacetonitrile.

High purity 2-naphthylacetonitrile and method for producing same

High purity 2-naphthylacetonitrile with fewer impurities can be used as a starting material or intermediate for synthesizing various pharmaceutical products, agricultural chemicals, and chemical products, and a production method thereof. A high purity 2-naphthylacetonitrile having an HPLC purity of 2-naphthylacetonitrile of not less than 95 area %, and containing naphthalene compounds represented by the formulas (a)-(j) at a content of a predetermined area % or below. A method for producing high purity 2-naphthylacetonitrile, may include: subjecting 2′-acetonaphthone to a Willgerodt reaction in the presence of an additive where necessary, and hydrolyzing the obtained amide compound to give 2-naphthylacetic acid; and reacting the 2-naphthylacetic acid obtained in the subjecting, a halogenating agent and sulfamide in the presence of a catalyst as necessary in an organic solvent to give 2-naphthylacetonitrile.

ACETONITRILE SEPARATION PROCESS

A process for producing acetonitrile, the process comprising dehydrating a feedstock stream comprising acetonitrile, acrylonitrile, allyl alcohol, and water (and optionally methanol) in a dehydration (first) column to yield a dehydrated acetonitrile stream comprising acetonitrile and acrylonitrile, less than 1 wt % allyl alcohol, and less than 50 wt % water, and optionally hydrogen cyanide; distilling the dehydrated acetonitrile stream in a lights (second) column to yield a distillate stream comprising lights, and a bottoms stream comprising acetonitrile, acrylonitrile, water, and optionally hydrogen cyanide and acrylonitrile; extracting the distillation bottoms stream in an extraction (third) column to yield a raffinate stream comprising acetonitrile and less than 200 ppm acrylonitrile and an extract stream comprising water and acrylonitrile; purifying the raffinate stream to yield a product acetonitrile stream.