Disclosed are methods for separating, recovering, and purifying cannabidiolic acid (CBDA) salts from an organic solvent solution comprising a mixture of cannabinoids. The methods comprise solubilizing the mixture of cannabinoids in C5-C7 hydrocarbon solvents, adding thereto a selected amine to thereby precipitate a CBDA-amine salt therefrom, dissolving the recovered CBDA-amine salt in a selected solvent and then adding thereto a selected antisolvent to thereby recrystallize a purified CBDA-amine salt therefrom. The recrystallized CBDA-amine salt may be decarboxylated to form a mixture of cannabidiol (CBD) and amine. The CBD amine mixture may be acidified to separate the amine from CBD. Also disclosed are CBDA-amine salts produced with certain amines selected from groups of secondary amines, tertiary amines, diamines, amino alcohols, amino ethers, and highly basic amines.

Disclosed are methods for separating, recovering, and purifying cannabidiolic acid (CBDA) salts from an organic solvent solution comprising a mixture of cannabinoids. The methods comprise solubilizing the mixture of cannabinoids in C5-C7 hydrocarbon solvents, adding thereto a selected amine to thereby precipitate a CBDA-amine salt therefrom, dissolving the recovered CBDA-amine salt in a selected solvent and then adding thereto a selected antisolvent to thereby recrystallize a purified CBDA-amine salt therefrom. The recrystallized CBDA-amine salt may be decarboxylated to form a mixture of cannabidiol (CBD) and amine. The CBD amine mixture may be acidified to separate the amine from CBD. Also disclosed are CBDA-amine salts produced with certain amines selected from groups of secondary amines, tertiary amines, diamines, amino alcohols, amino ethers, and highly basic amines.

This present invention provides gemcabene pharmaceutically acceptable salts having a PSD90 of 35 μm to about 90 μm, methods for purifying crude gemcabene, pharmaceutically acceptable salts of purified gemcabene, pharmaceutical compositions of a gemcabene pharmaceutically acceptable salt and therapeutic and prophylactic methods useful for various conditions, including dyslipidemia.

This present invention provides gemcabene pharmaceutically acceptable salts having a PSD90 of 35 μm to about 90 μm, methods for purifying crude gemcabene, pharmaceutically acceptable salts of purified gemcabene, pharmaceutical compositions of a gemcabene pharmaceutically acceptable salt and therapeutic and prophylactic methods useful for various conditions, including dyslipidemia.

The present disclosure belongs to the technical field of separation and purification of glycolic acid, and in particular, to a method and device for separation and purification of glycolic acid by a rectification-crystallization coupling process and use. Bio-based platform compound molecules are used as raw materials to synthesize the glycolic acid, and the obtained crude glycolic acid is separated and purified using the rectification-crystallization coupling process to obtain high-purity glycolic acid. The method initiates system separation and purification under a new glycolic acid synthesis route, which has the difficulty that the glycolic acid is easy to polymerize during concentration, so there are technical barriers to equipment design of vacuum rectification and adjustment of process parameters. In addition, during crystallization, there are technical barriers to equipment design of a crystallization kettle and adjustment of process parameters.

The present disclosure belongs to the technical field of separation and purification of glycolic acid, and in particular, to a method and device for separation and purification of glycolic acid by a rectification-crystallization coupling process and use. Bio-based platform compound molecules are used as raw materials to synthesize the glycolic acid, and the obtained crude glycolic acid is separated and purified using the rectification-crystallization coupling process to obtain high-purity glycolic acid. The method initiates system separation and purification under a new glycolic acid synthesis route, which has the difficulty that the glycolic acid is easy to polymerize during concentration, so there are technical barriers to equipment design of vacuum rectification and adjustment of process parameters. In addition, during crystallization, there are technical barriers to equipment design of a crystallization kettle and adjustment of process parameters.

The present disclosure belongs to the technical field of separation and purification of glycolic acid, and in particular, to a method and device for separation and purification of glycolic acid by a rectification-crystallization coupling process and use. Bio-based platform compound molecules are used as raw materials to synthesize the glycolic acid, and the obtained crude glycolic acid is separated and purified using the rectification-crystallization coupling process to obtain high-purity glycolic acid. The method initiates system separation and purification under a new glycolic acid synthesis route, which has the difficulty that the glycolic acid is easy to polymerize during concentration, so there are technical barriers to equipment design of vacuum rectification and adjustment of process parameters. In addition, during crystallization, there are technical barriers to equipment design of a crystallization kettle and adjustment of process parameters.

Methods of preparing a fenfluramine active pharmaceutical ingredient are provided. Aspects of the method include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to produce a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reductively aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with ethylamine using a borohydride reducing agent to produce a fenfluramine composition. Also provided are compositions and pharmaceutical ingredients prepared according to the subject methods including a pharmaceutically acceptable salt of fenfluramine and having less than 0.2% by weight in total of trifluoromethyl regioisomers.

Methods of preparing a fenfluramine active pharmaceutical ingredient are provided. Aspects of the method include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to produce a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reductively aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with ethylamine using a borohydride reducing agent to produce a fenfluramine composition. Also provided are compositions and pharmaceutical ingredients prepared according to the subject methods including a pharmaceutically acceptable salt of fenfluramine and having less than 0.2% by weight in total of trifluoromethyl regioisomers.

Methods of preparing a fenfluramine active pharmaceutical ingredient are provided. Aspects of the method include (a) hydrolyzing a 2-(3-(trifluoromethyl)phenyl)acetonitrile composition to produce a 2-(3-(trifluoromethyl)phenyl)acetic acid composition; (b) reacting the 2-(3-(trifluoromethyl)phenyl)acetic acid composition with acetic anhydride and a catalyst to produce a 1-(3-(trifluoromethyl)phenyl)propan-2-one composition; and (c) reductively aminating the 1-(3-(trifluoromethyl)phenyl)propan-2-one composition with ethylamine using a borohydride reducing agent to produce a fenfluramine composition. Also provided are compositions and pharmaceutical ingredients prepared according to the subject methods including a pharmaceutically acceptable salt of fenfluramine and having less than 0.2% by weight in total of trifluoromethyl regioisomers.