81results about How to "The amount of three wastes is less" patented technology

The invention discloses an industrial production process for tenofovir disoproxil fumarate represented by a structural formula (II). The production process comprises the following steps of: (1) preparing R-9-(2-hydroxypropyl)adenine by taking adenine and R-propylene carbonate as initial raw materials; (2) performing a condensation reaction on the obtained R-9-(2-hydroxypropyl)adenine and diethyl(tosyloxy)methylphosphonate under the catalytic action of magnesium alkoxide to prepare R-9[2-(diethyl-phosphonic acid methoxy)propyl]adenine; (3) hydrolyzing R-9[2-(diethyl-phosphonic acid methoxy)propyl]adenine to obtain tenofovir; and (4) performing condensation on the tenofovir and the chloromethyl isopropyl carbonate under the catalytic action of triethylamine to prepare the tenofovir disoproxil fumarate. The process of the invention has the characteristics of low cost, safe process, high product quality and suitability for industrial production.

The invention discloses a novel method of preparing 2-nitro-4-methylsulfonyl benzoic acid. The target product which is 2-nitro-4-methylsulfonyl benzoic acid is prepared by carrying out reaction by adopting an oxidation reaction device with a self-priming stirrer, wherein 2-nitro-4-methylsulfonyltoluene is used as the raw material, sulfuric acid is used as a reaction medium, a transition metal oxide is used as the catalyst, and oxygen is introduced in the course of reaction. The method provided by the invention has the advantage that the reaction condition is easy to control, the production cost is low, and the amount of the generated three wastes is reduced.

The invention provides a method for synthesizing dinitrile ethyl tertiary amine from aliphatic primary amine by a one-step method, which comprises the steps of adding aliphatic primary amine into acrylonitrile by using a glycollic acid aqueous solution as a catalyst, synthesizing a dinitrile ethyl tertiary amine compound by a one-step method under heating reflux, and after the reaction is finished, carrying out reduced pressure distillation treatment to remove low-boiling-point components, and obtaining the dinitrile ethyl tertiary amine compound with the yield being higher than 95%. The process provided by the invention has the following advantages: 1) single nitrile ethylation reaction and double nitrile ethylation reaction are carried out at the same time, so that the reaction efficiency is improved; 2) the glycollic acid is weak in acidity and basically has no corrosion to reaction equipment, so that the equipment investment is reduced; and 3) the reaction mother liquor does not need to be neutralized by adding alkali, so that a large amount of salt-containing wastewater is avoided, and the post-treatment process is simplified.

The invention discloses a synthesis method of a UV absorbent ethylhexyl triazone. The synthesis method comprises that melamine and 4-chlorobenzoic acid as initial raw materials undergo a trisubstitution reaction to produce 2,4,6-tris[(p-carboxyphenyl)amino]-1,3,5-triazine (H3TATAB), 2,4,6-tris[(p-carboxyphenyl)amino]-1,3,5-triazine (H3TATAB) and isooctanol undergo an esterification reaction to produce an ethylhexyl triazone crude product, the ethylhexyl triazone crude product is subjected to distillation desolvation and crystallization and the crystals are dried to form an ethylhexyl triazone finished product. The synthesis method has the characteristics of simple production route, easily available raw materials, mild reaction conditions, unique crystallization method, less three wastes and high product purity and is suitable for industrial production.

The invention relates to a synthetic method of 2,5-dichlorophenol, and belongs to the technical field of dicamba key intermediate synthesis. 1,2,4-trichlorobenzene generated by pure benzene chlorination can be easily separated from 1,4-dichlorobenzene to avoid high production cost and low production efficiency caused by difficulty in separation. Since the 1,2,4-trichlorobenzene and the 1,4-dichlorobenzene can independently obtain the 2,5-dichlorophenol, the use ratio of raw materials is high, the waste of a by-product is avoided, and therefore, the production cost is greatly lowered. In addition, the 1,4-dichlorobenzene can obtain the 2,5-dichlorophenol through two different methods. The synthetic method has the advantages of simple synthetic process, low production cost, high raw material use ratio, less process byproducts and small three-waste output and is more suitable for large-scale industrial production.

The invention relates to a bulk pharmaceutical chemical production technology, in particular to a novel rifamycin SV sodium salt production technology.A W/O emulsion liquid membrane is extracted from fermentation broth, and rifamycin SV sodium is directly generated.The content of the product obtained by means of the production technology is 90-97%, and water content is 2.6-5%.The technological process is short, three-waste output is low, raw material consumption is low, the yield of rifamycin SV sodium is effectively increased, and the problems of existing technologies that the technological process is long, impurity content is high and yield is low are solved.The novel rifamycin SV sodium salt production technology has great significance in promoting industrial development and has broad industrialized application prospects.

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 provides a preparation method of 4-phenylthiolthiophenol. The preparation method comprises the following steps: performing a bromination reaction on diphenyl sulfide and a bromination reagent to prepare 4-bromodiphenyl sulfide, performing a Grignard reaction on the obtained 4-bromodiphenyl sulfide to obtain a corresponding Grignard reagent, reacting the Grignard reagent with sulfur,and acidifying to prepare the 4-phenylthiolthiophenol. The method has the advantages of cheap and accessible raw materials, simple operation technique and low cost, can easily implement the reaction conditions, and is low in wastewater generation, safe, environment-friendly, high in atom economy, few in byproducts, high in yield and purity and suitable for industrial production.

The invention provides a preparation method of a 5,6-dihydropyridine-2 (1H)-one derivative, and particularly relates to a 1-(piperidine-2-keto-1-yl)-4-(5,6-dihydro-3-R substituent pyridine-2 (1H)-keto-1-yl) benzene preparation method, wherein the R substituent is chlorine or morpholine-4-yl. According to the invention, p-acetamido aniline is used as a raw material, and amidation with delta-valerolactone, halogenation with a halogenation reagent or sulfonylation with sulfonyl chloride, condensation, deacetylation, amidation with 2,2-dichloro-delta-valerolactone, halogenation with a halogenationreagent or sulfonylation with sulfonyl chloride, condensation elimination or condensation elimination substitution in the presence of morpholine are performed to obtain the target product. Accordingto the invention, the raw materials used in the preparation method are cheap, easy to obtain and low in cost; the process operation is simple, reaction conditions are easy to realize, the wastewater yield is low, and safety and greenness are realized; and the reaction selectivity of each step is high, the product yield and purity are high, and industrial production is facilitated.

The invention discloses a synthesis method of ethisterone which is prepared by adopting 4AD namely soybean oil tailings as a raw material, carrying out etherification protection as well as two-step reaction, namely, ethynylation and hydrolysis, and then refining. According to the invention, the raw material is replaced, that is the industrial tailing fermentation product 4AD of the soybean oil is used to replace diene; the raw material is wide in supply, low in cost and little in pollution; the reaction route is short; the process is simple; the auxiliary materials are commonly used chemical products; the generation amount of waste gas, waste water and waste solid is small and is a quarter of that generated in the traditional process.

The invention provides a buparvaquone preparation method, which comprises: carrying out condensation, hydrolysis and decarboxylation by using o-phthalic acid diester and 2-(4-tert-butylcyclohexylmethyl)succinic acid diester as a raw material to prepare 2-[(4-tert-butylcyclohexyl)methyl]-2,3-dihydro-1,4-naphthalenedione, carrying out a substitution reaction on the 2-[(4-tert-butylcyclohexyl)methyl]-2,3-dihydro-1,4-naphthalenedione and a halogenating reagent to obtain a dihalogenated compound mixture, removing halogen hydride through an elimination reaction to obtain 2-[(4-tert-butylcyclohexyl)methyl]-3-halo-1,4-naphthalenedione, and finally carrying out a hydrolysis reaction to obtain the buparvaquone (I). According to the invention, the method has advantages of cheap and easily available raw materials, safe and simple process operation, low cost, little wastewater generation, safety and environmental protection, easily achieved reaction conditions, stable reaction intermediate, high reaction activity, high selectivity and few side reactions, and the prepared buparvaquone is few in impurity and high in purity and yield.

The invention discloses a synthesis method of novaluron. P-nitrophenol is taken as a starting material, and hydrogen peroxide and hydrochloric acid chloro are used for preparing 2-chloro-4-nitrophenol; an inorganic base catalyst and perfluorinated vinyl methyl ether are used for addition reaction, 2-chloro-4-nitro-1-(1, 1, 2-trifluoro-2-(trifluoro methoxy) ethoxy) benzene is obtained, then nitro is reduced to obtain 3-chloro-4-(1, 1, 2-trifluoro-2-(trifluoro methoxy) ethoxy) aniline, and finally, 3-chloro-4-(1, 1, 2-trifluoro-2-(trifluoro methoxy) ethoxy) aniline reacts with 2, 6-difluorobenzoyl isocyanate to obtain novaluron. According to the method, raw materials are low in cost and easy to obtain, the operation is simple and convenient, the cost is low, the side reaction is few, and the method is suitable for industrial production.

The invention provides a simple and convenient preparation method of a 5,6-dihydropyridine-2(1H)-one derivative. The preparation method comprises the following steps: amidating p-phenylenediamine as araw material and delta-valerolactone, and reacting and condensing the hydroxyl of the obtained amidation product and a halogenating reagent 1 or sulfonyl chloride to obtain 1,4-bis(piperidine-2-keto-1-yl)benzene; carrying out carbonyl ortho-halogenation and elimination to obtain 1-(piperidine-2-keto-1-yl)-4-(5,6-dihydropyridine-2(1H)-keto-1-yl)benzene, and carrying out addition and elimination with a halogenating reagent 3 or carrying out elimination substitution in the presence of morpholine to obtain the 5,6-dihydropyridine-2(1H)-one derivative (I). The preparation method has the advantagesof cheap and easily available raw materials, short steps and low cost; the process operation is simple, reaction conditions are easy to realize, the wastewater yield is low, and safety and greennessare realized; and the reaction selectivity of each step is high, the product yield and purity are high, and industrial production is facilitated.