32 results about "Benzylamine hydrochloride" patented technology

The invention provides a porous material based on modified steel slag and a preparation method of the porous material. The porous material is prepared by mixing and sintering grinded and refined modified steel slag with coal ash, a pore-forming agent and clay, specifically, the preparation method comprises the following steps: dissolving calcium salt or sodium salt, polyhydric alcohol benzylamine hydrochloride into water so as to form a solution, mixing and stirring dihydric alcohol and an organic alkylol amine compound in sequence, finally adding glacial acetic acid, and uniformly mixing so as to obtain a grinding assisting activating agent; adding the grinding assisting activating agent into the steel slag, and performing high-speed ball milling in a ball mill so as to obtain grinded activated steel slag powder; uniformly mixing the grinded activated steel slag powder with the coal ash, moistening and aging with a small amount of water, adding sufficiently moistened polystyrene foam granules, further adding clay, uniformly mixing, pressing into round blanks, and performing high-temperature sintering, thereby obtaining the porous material based on the modified steel slag. As the modified steel slag which is small in granularity and high in activity is adopted as a raw material, the prepared porous material is moderate in porosity, high in mechanical strength and good in comprehensive property.

The invention belongs to the field of artificial synthesis of natural products and relates to an artificial synthesis method of a capsaicin homologue. The artificial synthesis method of the capsaicin homologue is to lead 4-hydroxy-3-methoxy-benzylamine hydrochloride to be reacted with the corresponding long-chain acid (E)-8-methyl-6-nonenoic acid and 8-methyl nonanoic acid or 7-methyl octanoic acid for preparing the capsaicin homologue. The long-chain acid synthesis method is characterized in that the method can avoid the use of triphenyl phosphine and other toxic substances which are commonly used in the existing patents and toxic substance-triphenyl phosphineoxide in byproducts, thereby being relatively environment-friendly. For different capsaicin homologues, the required starting raw materials are different. In particular, dihydrocapsaicin is applicable to large-scale industrial production.

The invention relates to a new preparation process of the medicinal raw material duloxetine hydrochloride of an antidepressant drug and belongs to the technical field of drug synthesis. The new preparation process is characterized in that N-methyl benzylamine hydrochloride but not dimethylamine hydrochloride is used in Mannich reaction; because benzyl is easier to remove as compared with methyl, dealkylation in a subsequent step has better effect and higher yield; an expensive chiral catalyst or a phase-transfer catalyst is not used; a better solvent crystallizing and removing method is adopted, so that the harm of a residual crystallizing solvent to a human body is prevented; the splitting of a chiral compound is carried out after dealkylation, and a mixture obtained after splitting is separated by adopting a unique recrystallization technology to prepare (S)-N-methyl-3-(1-naphthoxy)-3-(2-thienyl) propylamine/tartrate with high purity and high optical activity, so that a finally obtained duloxetine hydrochloride product can achieve better treatment effect. The new preparation process disclosed by the invention has the advantages of mildness in reaction condition, clear process, good easiness and convenience in operation and low production cost and is extremely favorable for industrial production.

The invention provides a method for preparing vilazodone hydrochloride midbody. The method comprises the steps of: based on 5-amino coumarone ethyl formate as an initial raw material, reacting with bi(2-chloroethy) benzylamine hydrochloride under the effect of tetrabutylammonium bromide to generate compound II, and reacting with ammonia to prepare compound I 5-(1-piperazinyl)-benzofuran-2-formamide. The used method is easy in raw material obtaining, low in cost, high in reaction yield, simple to operate and suitable for industrial production.

The invention discloses a preparation method of O-benzylhydroxylamine hydrochloride, and relates to the technical field of organic synthesis. The method comprises the following steps: synchronously dropwise adding alcoholic solutions of benzyl halide and alkoxide into oxime to perform a reaction; when no benzyl halide exists in the reaction system, carrying out solid-liquid separation, dropwise adding dilute hydrochloric acid for carrying out hydrolytic rectification, and distilling while dropwise adding the dilute hydrochloric acid to separate out ketone; concentrating the reaction solution and separating out O-benzylhydroxylamine hydrochloride; and drying the benzylamine hydrochloride to obtain an O-benzylhydroxylamine hydrochloride pure product. Oxime is used as a raw material, and thefinally generated ketone or aldehyde can also be recycled to synthesize corresponding oxime. According to the method, the atom utilization rate is improved, the production cost of the product is reduced, the emission of three wastes is reduced, and the goal of green production is achieved.

The invention discloses a preparation method of tetraimidazole free alkali. Alpha-[[(2-hydroxyethyl)amino]methyl]benzyl alcohol reacts with thionyl chloride, then water is added for heating dissolution, after activated carbon thermal filtration, N-(2-chloroethyl)-alpha-(chloromethyl)-benzylamine hydrochloride is obtained through cooling crystallization, then N-(2-chloroethyl)-alpha-(chloromethyl)-benzylamine hydrochloride and thiourea are subjected to direct cyclization, and tetraimidazole free alkali is generated. The method is simple in production process, mild in reaction condition and highin total yield, the production cost is reduced, the generation amount of three wastes is small, the double contradiction between economy and environment in the development process of modern enterprises is well solved, and the production process has great competitiveness and good industrial prospects.

The invention relates to a synthetic method of snake venom-like tripeptide, which comprises the following steps: by taking 3-phthalimidopropionic acid as an initial raw material, performing acylating chlorination, condensing with proline, and condensing an obtained fragment with L-2, 4-diaminobutyryl benzylamine hydrochloride with a side chain protected by phthaloyl, thereby obtaining the phthaloyl-protected snake venom-like tripeptide. Finally, a phthaloyl protecting group is removed through hydrazine, and then the free snake venom-like tripeptide is obtained. The free snake venom-like tripeptide is obtained after a phthaloyl protecting group is removed by hydrazine, and can be conveniently prepared into acetate and hydrochloride products. Compared with the prior art, the method has the advantages of easily available raw materials, high product purity, simplicity and convenience in operation and suitability for industrial production.

The invention provides a preparation method of tetraimidazole hydrochloride, which comprises the following steps: preparing tetraimidazole; the preparation method comprises the following step: reacting tetraimidazole, 1, 2-dibromoethyl benzene and 2-aminothiazoline hydrochloride to generate tetraimidazole. The synthetic route is shorter, the comprehensive yield is higher than that of other processroutes, styrene is used as an initiator, tetra-imidazole free alkali is used as a final product, the yield of the hydroxysalt process route is about 65%, the yield of the N (2chloroethyl) alpha (chloromethyl) benzylamine hydrochloride process route is about 72%, and the yield can reach 85% or above when the patent route is used. Meanwhile, the problem of large amount of waste water and waste saltgenerated by multi-step reactions such as chlorination, hydrolysis and cyclization is avoided, the investment of reaction equipment such as an autoclave is avoided, the green chemical engineering requirement is met, the economic benefit is remarkable, and the industrial prospect is good.

The invention provides a preparation method of an Avanafil intermediate. The preparation method comprises the following steps: dissolving 4-hydroxy-2-methylthio-ethyl 5-pyrimidinecarboxylate and potassium carbonate in DMF to obtain a mixed solution, adding methanesulfonyl chloride into the mixed solution under the stirring condition, continuously stirring after addition until a reaction is ended, adding water and ethyl acetate into a reaction solution, carrying out extraction and liquid separation, carrying out vacuum concentration on an organic phase to prepare 4-methanesulfonic sulfonic ester-2-methylthio-ethyl 5-pyrimidinecarboxylate; dissolving the obtained 4-methanesulfonic sulfonic ester-2-methylthio-ethyl 5-pyrimidinecarboxylate into DMF, adding a (3-chloro-4-methoxy)Benzylamine hydrochloride to obtain mixed liquor, adding triethylamine into the mixed liquor under the stirring condition, continuously stirring after addition until a reaction is ended, adding water and ethyl acetate, carrying out extraction and liquid separation, carrying out vacuum concentration on an organic phase, and recrystallizing to prepare 4-(3-chloro-4-methoxybenzylamino)-5- ethyloxycarbonyl-2-methylthiopyrimidine. The invention has advantages of less environmental pollution, high product yield, safe post-processing and simple operation.

The invention discloses a novel method for preparing N-[4-[1-hydroxy-2-[(1-methylethyl)amino]ethyl]methylsulfonyl benzylamine hydrochloride (I), which comprises: reaction of phenylamine and methanesulfonyl chloride to produce N-phenyl methanesulfonamide (II), reaction of the obtained compound (II) and chloroacetyl chloride to produce N-[4-[2-chloroacetyl phenyl]methanesulfonamide (III), reaction of the obtained compound (III) and isopropamide to produce N-[4-[2-(1-methylethyl)amino]acetyl]methylsulfonyl benzylamine hydrochloride (VI), and reduction of the obtained compound (VI) by sodium borohydride to produce the target product N-[4-[1-hydroxy-2-[(1-methylethyl)amino]ethyl]methylsulfonyl benzylamine hydrochloride (I). The method has the advantages of low cost, short reaction procedures, simple operation, high yield, high product purity and the like, and is suitable for industrial production.

The invention discloses a method for preparing a microsomal prostaglandin E2 synthase-1 inhibitor. The method comprises the following three steps: 1) preparing N-substituted amide from 5-iodoisatoic anhydride and 4-(3-chlorophenyl)benzylamine hydrochloride; 2) reacting N-substituted amide with crotonyl alcohol to produce 3-[(3'-chloro[1,1'-diphenyl]-4-yl)methyl]-2-propyl-6-iodoquinazolinone; and 3) subjecting a reaction product of the previous step and the o-chlorobenzamide to a Goldberg amination reaction to obtain the target product. The preparation method is simple in steps, avoids the useof alkali and toxic chemical reagents such as triphenyl phosphite, uses cheap and readily-available crotonyl alcohol as a raw material, realizes automatic transferring of hydrogen, does not use alkaliduring the reaction, achieves one-pot reaction, only by-produces water, has high atom economy in the reaction, meets the requirements of green chemistry and shows good development prospects.

The invention belongs to the technical field of medical intermediates, and particularly relates to a synthesis method of 2-fluoro-3-methyl-4-(trifluoromethyl) benzylamine hydrochloride. A compound A and a compound E are used as initial raw materials for the first time to form a compound B, then the compound B is subjected to a reaction to form a compound C, and the compound C is used for preparingthe 2-fluoro-3-methyl-4-(trifluoromethyl) benzylamine hydrochloride.

The present invention relates to a novel polymorphic form of N-[2-(6-fluoro-1H-indol-3-yl)ethyl]-3-(2,2,3,3-tetrafluoropropoxy)benzylamine hydrochloride.