40 results about "4-Chloroaniline" patented technology

The invention provides transformation method for poly-halogenated aromatic amine compound. In the method, a hydrodechlorination reaction is carried out on the poly-chloraniline compound (I) rich in the rectification residue, with the existence of H2, liquid solvent and alkali, by taking the rectification residue generated in the process of synthesizing 2, 5 dimethoxy-4-chloraniline as raw materials and by adopting a support catalyst with group VIII metals as active components. The method has the advantage that the rectification residue generated in the process of synthesizing 2, 5 dimethoxy-4-chloraniline can be recycled at utmost, so that the environmental pollution caused by the discharge of rectification residue is reduced.

The invention discloses a synthetic method for 4-chlorophenylhydrazine hydrochloride. The synthetic method comprises the following steps: 4-bromochlorobenzene and hydrazine hydrate are taken as reaction raw materials, and a phase transfer catalyst, a solvent and a catalyst are added for a reaction; after the reaction, solids are filtered and separated, and a solvent is removed from a filtrate through distillation; hydrochloric acid is added to residues obtained after distillation, and the mixture is stirred and filtered; filter residues are washed with water and dried, and 4-chlorophenylhydrazine hydrochloride is obtained. The synthetic method aims to solve the problem of generation of a large amount of wastewater due to adoption of a current commonly used method for reduction acidification after diazotization of 4-chloroaniline, 4-bromochlorobenzene and hydrazine hydrate are taken as the reaction raw materials, the phase transfer catalyst, the solvent and the catalyst are added for the reaction, the reaction steps are simple, the wastewater produced in a 4-chlorophenylhydrazine synthetic method is reduced remarkably, sulfur dioxide is prevented from being produced through reduction of sodium sulfite, excessive hydrazine hydrate and solvent can be recovered and reused after reaction, and the method is environment-friendly.

The invention discloses a method for preparing known impurities of gefitinib, comprising: mixing initial raw materials: 2-amino-4-methoxy-5-(3-morpholine propanolato) cyanophenyl, 3-fluorine-4-chloroaniline and acetate solvent with trimethyl orthoformate or triethyl orthoformate, simply preparing a crude product of the impurities of gefitinib, and recrystallizing to obtain the high purity known impurities of gefitinib, that is N-(4-chloro-3-fluorophenyl)-7-methoxy-6-(3-morpholinopropoxy)quinazolin-4-amine. The method has advantages of short synthesis route, simple operation, and high purity of obtained product, and can be used for reference substance research.

The invention discloses a synthetic method for 4-chlorophenylhydrazine hydrochloride. The synthetic method comprises the following steps: 4-bromochlorobenzene and hydrazine hydrate are taken as reaction raw materials, and a phase transfer catalyst, a solvent and a catalyst are added for a reaction; after the reaction, solids are filtered and separated, and a solvent is removed from a filtrate through distillation; hydrochloric acid is added to residues obtained after distillation, and the mixture is stirred and filtered; filter residues are washed with water and dried, and 4-chlorophenylhydrazine hydrochloride is obtained. The synthetic method aims to solve the problem of generation of a large amount of wastewater due to adoption of a current commonly used method for reduction acidification after diazotization of 4-chloroaniline, 4-bromochlorobenzene and hydrazine hydrate are taken as the reaction raw materials, the phase transfer catalyst, the solvent and the catalyst are added for the reaction, the reaction steps are simple, the wastewater produced in a 4-chlorophenylhydrazine synthetic method is reduced remarkably, sulfur dioxide is prevented from being produced through reduction of sodium sulfite, excessive hydrazine hydrate and solvent can be recovered and reused after reaction, and the method is environment-friendly.

The invention discloses a 3,5-disubsitutued 2-amino-pyrazine compound. The compound has the structure shown in the formula I; in the formula I, NR1R2 is n-propylamino, cyclopropylamino, cyclopentylamino, cyclohexylamino, morpholinyl, 4-methyl piperazine, anilino, 4-chloroaniline or 3-chloroaniline; Ar is 3,5-dimethyl-isoxazolyl-4 or 1-methyl-1H-pyrazolyl-4; and the invention further provides the preparation technology and application thereof. The compound has the outstanding inhibiting effect on growth of four kinds of cancer cells including a human cervical cancer cell HeLa, a human brain glioma cell U87, a human hepatoma cancer cell HepG2 and a human colon cancer cell LoVo, wherein a large part of the compound has an obviously higher inhibiting effect on proliferation of the cancer cellsthan positive control VX-680, particularly the compound Ih and Ii have relatively high activity on the four kinds of cancer cells, and have prominent activity inhibiting effect on aurora kinase A andaurora kinase B, and therefore the compound can be applied to preparation of anti-cancer drugs.

The invention provides a Pd complex catalyst as well as a preparation method and application thereof. The Pd metal complex catalyst provided by the invention has the structure shown by a formula (I), wherein R1 and R2 are alkyls or halogens; preferably, R1 is alkyl with 1-15 carbons, and R2 is alkyl with 1-5 carbons, or halogen; more preferably, R1 is methyl, ethyl, propyl or benzhydryl, and R2 is methyl or chlorine. DBCPh-NH2 is 2,6-bi (diphenylmethyl)-4-chloroaniline. According to the Pd metal complex catalyst, Heck reaction can be promoted when less Pd metal complex catalyst is used; and furthermore, the Pd metal complex catalyst has good catalytic performance and can be used for realizing the catalysis for the Heck reaction.

The invention discloses a drug intermediate of halofuginone and a synthesis method of a halofuginone parent nucleus. The structural formula of the intermediate is disclosed in the specification. The synthesis method of the halofuginone parent nucleus is characterized by comprising the following steps: 1) in the presence of a catalyst, heating 3-bromo-4-chloroaniline and trimethyl orthoformate to sufficiently react, cooling, sufficiently reacting with NH3, separating, and carrying out primary purification to obtain a solid crude product; and 2) in the presence of a catalyst, sufficiently heating the obtained solid, acetic acid, CO and O2 to react, separating and purifying to obtain the end product. The synthesis method is a two-step process, and has the advantages of simple technique, environment friendliness, high yield and very low cost since the raw materials are accessible 3-bromo-4-chloroaniline and trimethyl orthoformate.

The invention belongs to the organic synthesis field, and specifically relates to a synthetic method of 7-chloro-1,2,3,4-tetrahydrobenzo[b]azepine-5-one. According to the invention, the technical problems to be solved are low yield, high cost and difficult after-treatment purification of the existing synthetic method; a technical scheme for solving the technical problems is to provide a synthetic method of 7-chloro-1,2,3,4-tetrahydrobenzo[b]azepine-5-one; the synthetic method comprises the following steps of: carrying out an acylation reaction between 4-chloroaniline and succinic anhydride to obtain 4-(4-chloroaniline)-4-oxobutyric acid; carrying out an intramolecular Friedel-Craft reaction on 4-(4-chloroaniline)-4-oxobutyric acid to obtain 7-chloro-3,4-tetrahydrobenzo[b]azepine-2,5-one; reacting 7-chloro-3,4-tetrahydrobenzo[b]azepine-2,5-one with ethylene glycol to obtain 7-chloro-3,4-tetrahydrobenzo[b]azepine-2-one-5-glycol ketal; reducing 7-chloro-3,4-tetrahydrobenzo[b]azepine-2-one-5-glycol ketal, and carrying out de-ketalation under an acidic condition to obtain 7-chloro-1,2,3,4-tetrahydrobenzo[b]azepine-5-one. The invention provides a new method which is short in steps and high in total yield.

The invention provides a synthetic method of hexamethylene flusulfamide. The synthetic method comprises the following steps: reacting to obtain 2-oxocyclohexyl ammonium sulphonate and ammonium sulfate by adopting cyclohexanone, 1, 4-dioxane, sulfur trioxide and ammonia as the raw materials; washing via reaction product through absolute methanol, and leaching to separate ammonium sulfate; and then carrying out reaction among 2-oxocyclohexyl ammonium sulphonate, oxalyl chloride and 2-trifluoromethyl-4-chloroaniline to obtain hexamethylene flusulfamide. According to the synthetic method provided by the invention, KOH solution is replaced via the ammonia, thus, the reaction endpoint is easily controlled; the byproduct ammonium sulfate can be used as chemical fertilizer after being separated, and the generation of three wastes such as waste barium sulfate can be removed; the reaction is easy to operate, the post-processing is simple to carry out, the product is high in purity and high in yield, and the method is suitable for large-scale industrial application.