Process for the production of 2-dimethylaminoethyl (meth)acrylate in multiple stage batch reactions involving the recycling of the catalyst (DBTO) in subsequent reaction, the addition a certain amount of fresh catalyst to the recycled catalyst, the use of said catalysts in the subsequent reaction, and wherein the volume decrease due to azeotropic distillation is compensate in order to keep the volume constant in the reactor during the reaction by the continuous addition of a composition comprising methyl(meth)acrylate and dimethylaminoethanol.

The present invention is directed to a method of producing active pharmaceutical ingredients (APIs). The method includes subjecting a reaction mixture with an API precursor to solvent extraction to produce a reactant stream with the API precursor. The method includes concentrating the API precursor in the reactant stream using at least one membrane. The method includes carrying out a reaction in a membrane reactor. The method includes separating the API precursor from the reaction stream using a separator. The method includes crystallizing the API precursor using a crystallizer to produce APIs.

The present invention is directed to a method of producing active pharmaceutical ingredients (APIs). The method includes subjecting a reaction mixture with an API precursor to solvent extraction to produce a reactant stream with the API precursor. The method includes concentrating the API precursor in the reactant stream using at least one membrane. The method includes carrying out a reaction in a membrane reactor. The method includes separating the API precursor from the reaction stream using a separator. The method includes crystallizing the API precursor using a crystallizer to produce APIs.

A composition comprising a) a quaternary trialkylalkanolamine hydroxide and b) at least one diamine as component b), which is selected from the group consisting of 1-amino-4-methylpiperazine, 1,2-diaminopropane and mixtures thereof.

A composition comprising a) a quaternary trialkylalkanolamine hydroxide and b) at least one diamine as component b), which is selected from the group consisting of 1-amino-4-methylpiperazine, 1,2-diaminopropane and mixtures thereof.

Disclosed is a crystal form of dezocine. The X-ray powder diffraction (XRD) pattern thereof is determined using Cu/K-1 and has diffraction peaks at the 2 value of 9.10.2 and 12.20.2, with the height % of these diffraction peaks greater than 20. Also disclosed are a preparation method for the crystal form, a pharmaceutical composition and use thereof. The crystal form of dezocine has good solubility, the preparation method has simple operations, good reproducibility, suitability for industrial production and the like.

Disclosed is a crystal form of dezocine. The X-ray powder diffraction (XRD) pattern thereof is determined using Cu/K-1 and has diffraction peaks at the 2 value of 9.10.2 and 12.20.2, with the height % of these diffraction peaks greater than 20. Also disclosed are a preparation method for the crystal form, a pharmaceutical composition and use thereof. The crystal form of dezocine has good solubility, the preparation method has simple operations, good reproducibility, suitability for industrial production and the like.

A method for synthesizing 2-(2-aminoethoxy) ethanol, including the steps of producing 2-(2-phthalimidoethoxy) ethanol by reacting 5-tosyloxy-3-oxapentanol with potassium phthalate and converting the 2-(2-phthalimidoethoxy) ethanol to the 2-(2-aminoethoxy) ethanol by reacting the 2-(2-phthalimidoethoxy) ethanol with hydrazine monohydrate. Reacting the 2-(2-phthalimidoethoxy) ethanol with the hydrazine monohydrate may include forming a final mixture by adding the hydrazine monohydrate to a solution of 2-(2-phthalimidoethoxy) ethanol, refluxing the final mixture in a nitrogen atmosphere, extracting a second organic phase containing the 2-(2-aminoethoxy) ethanol from the final mixture using a second portion of chloroform, and purifying the 2-(2-aminoethoxy) ethanol from the second organic phase.

A method for synthesizing 2-(2-aminoethoxy) ethanol, including the steps of producing 2-(2-phthalimidoethoxy) ethanol by reacting 5-tosyloxy-3-oxapentanol with potassium phthalate and converting the 2-(2-phthalimidoethoxy) ethanol to the 2-(2-aminoethoxy) ethanol by reacting the 2-(2-phthalimidoethoxy) ethanol with hydrazine monohydrate. Reacting the 2-(2-phthalimidoethoxy) ethanol with the hydrazine monohydrate may include forming a final mixture by adding the hydrazine monohydrate to a solution of 2-(2-phthalimidoethoxy) ethanol, refluxing the final mixture in a nitrogen atmosphere, extracting a second organic phase containing the 2-(2-aminoethoxy) ethanol from the final mixture using a second portion of chloroform, and purifying the 2-(2-aminoethoxy) ethanol from the second organic phase.

A method for synthesizing 2-(2-aminoethoxy) ethanol, including the steps of producing 2-(2-phthalimidoethoxy) ethanol by reacting 5-tosyloxy-3-oxapentanol with potassium phthalate and converting the 2-(2-phthalimidoethoxy) ethanol to the 2-(2-aminoethoxy) ethanol by reacting the 2-(2-phthalimidoethoxy) ethanol with hydrazine monohydrate. Reacting the 2-(2-phthalimidoethoxy) ethanol with the hydrazine monohydrate may include forming a final mixture by adding the hydrazine monohydrate to a solution of 2-(2-phthalimidoethoxy) ethanol, refluxing the final mixture in a nitrogen atmosphere, extracting a second organic phase containing the 2-(2-aminoethoxy) ethanol from the final mixture using a second portion of chloroform, and purifying the 2-(2-aminoethoxy) ethanol from the second organic phase.