C07C233/03

RAPID SYNTHESIS METHOD FOR BIOMASS-BASED AMINE

A rapid synthesis method for a biomass-based amine, including: using formamide as an amine source, formic acid as a hydrogen source, and biomass aldehyde or ketone as a raw material, conduct rapid heating promoting direct addition of formamide and aldehyde or ketone compound through microwave-assisted heating and without a solvent and catalyst, and carrying out formic acid reduction preparing and obtaining a corresponding formamide derivative; selectively converting the formamide derivative under the action of a base into a corresponding primary amine through alcoholysis. The microwave-assisted heating reaction system has a significantly higher catalytic efficiency than a corresponding oil bath system, greatly shortens a reaction time, and significantly improves selectivity, where a conversion rate of a biomass aldehyde or ketone compound may reach at least 99%, and a formamide derivative yield may reach 85-99%; the formamide derivative is synthesized to a primary amine through alcoholysis, where a yield may reach 92-99%.

RAPID SYNTHESIS METHOD FOR BIOMASS-BASED AMINE

A rapid synthesis method for a biomass-based amine, including: using formamide as an amine source, formic acid as a hydrogen source, and biomass aldehyde or ketone as a raw material, conduct rapid heating promoting direct addition of formamide and aldehyde or ketone compound through microwave-assisted heating and without a solvent and catalyst, and carrying out formic acid reduction preparing and obtaining a corresponding formamide derivative; selectively converting the formamide derivative under the action of a base into a corresponding primary amine through alcoholysis. The microwave-assisted heating reaction system has a significantly higher catalytic efficiency than a corresponding oil bath system, greatly shortens a reaction time, and significantly improves selectivity, where a conversion rate of a biomass aldehyde or ketone compound may reach at least 99%, and a formamide derivative yield may reach 85-99%; the formamide derivative is synthesized to a primary amine through alcoholysis, where a yield may reach 92-99%.

DMF RECYCLING METHOD
20230295074 · 2023-09-21 ·

The invention provides a DMF recycling method, the method comprises: neutralization step, extraction and crystallization step, layering step, evaporation step; a condensate obtained by evaporation of the upper layer liquid phase is recycled into the anti-solvent, a concentrated solution obtained by evaporation of the upper layer liquid phase and a condensate obtained by evaporation of the lower layer liquid phase are mixed to obtain a crude DMF solution for recycling of DMF. The recycling method overcomes the problem that acetic acid in the stock solution corrodes the equipment and produces impurities, so as to improve the recycling purity and reduce the equipment cost.

DMF RECYCLING METHOD
20230295074 · 2023-09-21 ·

The invention provides a DMF recycling method, the method comprises: neutralization step, extraction and crystallization step, layering step, evaporation step; a condensate obtained by evaporation of the upper layer liquid phase is recycled into the anti-solvent, a concentrated solution obtained by evaporation of the upper layer liquid phase and a condensate obtained by evaporation of the lower layer liquid phase are mixed to obtain a crude DMF solution for recycling of DMF. The recycling method overcomes the problem that acetic acid in the stock solution corrodes the equipment and produces impurities, so as to improve the recycling purity and reduce the equipment cost.

METHOD FOR PREPARING FORMAMIDE COMPOUNDS VIA HYDROGENATION OF CARBON DIOXIDE CATALYZED BY POROUS MATERIALS
20220289666 · 2022-09-15 ·

A method for preparing formamide compounds via hydrogenation of carbon dioxide catalyzed by porous materials includes the following steps: by taking porous organometallic polymers as catalysts, reacting amine compounds with carbon dioxide and hydrogen under an air atmosphere to prepare formamide compounds. The method has the advantages of high reaction efficiency, good selectivity, mild conditions, economy, environmental protection, and simple operation. The catalysts are solid organometallic polymers with large specific surface area, strong carbon dioxide adsorption, hierarchical pore distribution, and uniformly dispersed metal centers. They are designed and synthesized as the reaction catalysts by changing the proportion of the cross-linked comonomer. The catalysts can be especially used for catalytic synthesis of fine chemical N, N-dimethylformamide (DMF) without addition of any additional solvent, alkali, or other additives, which is convenient for separation and purification of DMF.

METHOD FOR PREPARING FORMAMIDE COMPOUNDS VIA HYDROGENATION OF CARBON DIOXIDE CATALYZED BY POROUS MATERIALS
20220289666 · 2022-09-15 ·

A method for preparing formamide compounds via hydrogenation of carbon dioxide catalyzed by porous materials includes the following steps: by taking porous organometallic polymers as catalysts, reacting amine compounds with carbon dioxide and hydrogen under an air atmosphere to prepare formamide compounds. The method has the advantages of high reaction efficiency, good selectivity, mild conditions, economy, environmental protection, and simple operation. The catalysts are solid organometallic polymers with large specific surface area, strong carbon dioxide adsorption, hierarchical pore distribution, and uniformly dispersed metal centers. They are designed and synthesized as the reaction catalysts by changing the proportion of the cross-linked comonomer. The catalysts can be especially used for catalytic synthesis of fine chemical N, N-dimethylformamide (DMF) without addition of any additional solvent, alkali, or other additives, which is convenient for separation and purification of DMF.

HYBRID PEROVSKITE MATERIAL PROCESSING
20220187695 · 2022-06-16 ·

A method for preparing photoactive perovskite materials. The method comprises the steps of: introducing a lead halide and a first solvent to a first vessel and contacting the lead halide with the first solvent to dissolve the lead halide to form a lead halide solution, introducing a Group 1 metal halide a second solvent into a second vessel and contacting the Group 1 metal halide with the second solvent to dissolve the Group 1 metal halide to form a Group 1 metal halide solution, and contacting the lead halide solution with the Group 1 metal halide solution to form a thin-film precursor ink. The method further comprises depositing the thin-film precursor ink onto a substrate, drying the thin-film precursor ink to form a thin film, annealing the thin film; and rinsing the thin film with a salt solution.

Hybrid perovskite material processing

A method for preparing photoactive perovskite materials. The method comprises the steps of: introducing a lead halide and a first solvent to a first vessel and contacting the lead halide with the first solvent to dissolve the lead halide to form a lead halide solution, introducing a Group 1 metal halide a second solvent into a second vessel and contacting the Group 1 metal halide with the second solvent to dissolve the Group 1 metal halide to form a Group 1 metal halide solution, and contacting the lead halide solution with the Group 1 metal halide solution to form a thin-film precursor ink. The method further comprises depositing the thin-film precursor ink onto a substrate, drying the thin-film precursor ink to form a thin film, annealing the thin film; and rinsing the thin film with a salt solution.

Complex and method for producing same

A complex has a structure of formula (1A): SnX.sub.n.Math.(m)L, wherein X is at least one type of halogen atoms, L is a polar solvent molecule, n is a value from 1.5 to 2.5, and m is a value from 0.3 to 1.9. A perovskite compound has a structure of formula (2A): RSnX.sub.j, wherein Sn has an oxidation number from 1.5 to 2.5, R is at least one type of a monovalent cation, X is at least one type of halogen atoms, and j is a value from 2.5 to 3.5, and the perovskite compound is free of tin oxide; or a perovskite compound has a structure of formula (2B): R.sub.2M.sup.2BiX.sub.1, wherein R is at least one type of a monovalent cation, X is at least one type of halogen atoms; M.sup.2 is a monovalent metal, and i is a value from 5.0 to 7.0.

PROCESS FOR THE PREPARATION OF 6-(CYCLOPROPANEAMIDO)-4-((2-METHOXY-3-(1-METHYL-1H-1,2,4-TRIAZOL-3-YL)PHENYL)AMINO)-N-(METHYL-D3)PYRIDAZINE-3-CARBOXAMIDE

The invention relates to an improved process for synthesizing 6-(cyclopropaneamido)-4-((2-methoxy-3-(1-methyl-1H-1,2,4-triazol-3-yl)phenyl)amino)-N-(methyl-d3)pyridazine-3-carboxamide of the formula:

##STR00001##

Compound I is currently in clinical trials for the treatment of auto-immune and auto-inflammatory diseases such as psoriasis.