7 results about "Cycleanine dimethobromide" patented technology

The application discloses a synthesis method of 3-aminomethyl-3,5,5-trimethylcyclohexylamine. The method comprises the following steps: 1) taking 3-cyano-3,5,5-trimethylcyclohexylimine and hydrogen as raw materials, and performing imine hydrogenation reaction in a solvent in the presence of a first catalyst and a first cocatalyst to obtain 3-cyano-3,5,5-trimethylcyclohexylamine; 2) taking 3-cyano-3,5,5-trimethylcyclohexylamine and hydrogen as raw materials, and performing cyano hydrogenation reaction in an organic solvent in the presence of a second catalyst and a second cocatalyst to obtain a target product; the first catalyst contains one or both of nickel and cobalt; the first cocatalyst is a substance capable of reacting with hydrogen cyanide; the second catalyst contains iron; and the second cocatalyst is a Lewis acid catalyst. The synthesis method can obviously improve the yield and purity of the target product, the catalyst is more stable, the cost is lower, and the synthesis method is more environmentally friendly.

This invention relates to the field of pharmaceutical analysis technology, and provides a method for detecting N-methylcyclohexylamine hydrochloride in bromhexine hydrochloride. The method involves dissolving N-methylcyclohexylamine in an organic solvent as a reference solution, and dissolving bromhexine hydrochloride in an organic solvent containing an acid-binding agent as the test solvent, followed by headspace gas chromatography for detection. This method is simple, efficient, specific, sensitive, repeatable, and stable, and can be used for the quality control of bromhexine hydrochloride raw material, providing technical support for its production.

This invention discloses a method for synthesizing bromhexine hydrochloride, with the following specific steps: Step (1), using 2-amino-3,5-dibromobenzoic acid as a raw material, reacting it with trimethylacetyl chloride via an anhydride method under the action of an acid-binding agent to obtain compound 2-amino-3,5-dibromobenzoic acid anhydride; Step (2), the 2-amino-3,5-dibromobenzoic acid anhydride obtained in Step 1 undergoes nucleophilic addition with N-methylcyclohexylamine to obtain compound 5, bromhexine hydrochloride intermediate; Step (3), the above compound 5, bromhexine hydrochloride intermediate undergoes amide reduction and salt formation reaction to obtain bromhexine hydrochloride. This process provides a new route for preparing bromhexine hydrochloride, avoiding the heavily regulated chlorination process, reducing the release of toxic gases from strong halogen reagents such as thionyl chloride, significantly reducing safety risks and environmental protection investment, and the reaction itself is safe and fast, which is conducive to industrial production.

The application discloses a preparation method of N,N-dimethylcyclohexylamine with improved storage stability, which comprises the following steps: reacting cyclohexylamine, N,N-dimethylcyclohexylamine, formaldehyde and hydrogen under the action of a supported palladium-based catalyst; in the raw materials, the addition amount of N,N-dimethylcyclohexylamine is 1-5% of the mass of the cyclohexylamine, preferably 2-3%. The N,N-dimethylcyclohexylamine can be prepared at a high yield by the method, and the content of N-cyclohexylformamide impurities can be controlled to be below 10 ppm, and it is found that the low-temperature storage stability is significantly improved.

The embodiment of the invention provides a preparation method of N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide, atomized liquid and an atomization device, pentafluorobenzoic acid and 2-methylcyclohexyl amine can be subjected to a synthetic reaction in an organic solvent under the action of an alkaline substance and a condensing agent to generate N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide, and the atomized liquid is used for preparing N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide. The method comprises the following steps: dissolving a target product crude product of N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide into ethanol, filtering in a second mixed solution, dissolving in ethanol, decolorizing with activated carbon, carrying out hot filtration, adding water into a filtrate to precipitate a solid, filtering, and drying filter residues, thereby obtaining N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide with the purity of greater than or equal to 99%, namely N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide with the purity of greater than or equal to 99%. The method can effectively solve the problem that high-purity N-(2-methylcyclohexyl)-2, 3, 4, 5, 6-pentafluorobenzamide cannot be effectively synthesized in the prior art.

Thermoresponsive, switchable-hydrophilicity amine solvents such as diisopropylamine (DIPA), N,N-dimethylcyclohexylamine (DMCHA), dipropylamine (DPA), N-ethylcyclohexylamine (ECHA), triethylamine (TEA), and tert-octylamine (TOA) are used to extract lithium from hypersaline brines. The solvent is mixed with hypersaline brines containing lithium and other alkali metal cations at an extraction temperature. The result is a multi-phase mixture including a light, organic extract phase above a heavy, aqueous raffinate phase. Water and salt partitions from the aqueous phase into the organic phase, and lithium is preferentially partitioned over other alkali metal cations, enabling ion-specific separation. The extract is separated from the raffinate and warmed to a disengagement temperature. At higher temperatures, phase disengagement occurs as the substantially all previously extracted ions and water demix from the organic phase, yielding an aqueous product water stream containing the extracted cations and enriched with lithium. The regenerated solvent can be recycled for use in treatment of additional feed brine.

The present application relates to a kind of preparation methods of 3-aminomethyl-3,5,5-trimethylcyclohexane.The preparation method includes: isophorone nitrile, ammonia and hydrogen peroxide occur in the presence of modified titanium silicon catalyst and generate intermediate 1, and the obtained intermediate 1 occurs in the presence of hydrogenation catalyst and hydrogenation reaction generates 3-aminomethyl-3,5,5-trimethylcyclohexylamine.The method described in the present application can be operated at lower reaction pressure, reaction step is simple, yield is high, product is easy to purify and separate, and is suitable for industrial production.