111128-12-2Relevant articles and documents
Method for synthesizing P-bromomethyl isobenzopropionic acid
-
, (2021/10/27)
The invention provides a method for synthesizing p-bromomethyl isobenzopropionic acid, and relates to the technical field of organic synthesis. The synthesis method disclosed by the invention comprises the synthesis of isobenzoates. Vilsmeier Reagent preparation method comprises the following steps: synthesizing aldehyde isopropylparaben, synthesizing methyl isopropylbenzene, separating and purifying bromomethyl isobenzopropionic acid and, and the like. The final para-position selectivity of the method can reach 90 - 97%, and the three-waste yield is greatly reduced.
Production method of 2-(4-bromomethyl phenyl)propionic acid
-
Paragraph 0017; 0022; 0028; 0029, (2020/03/06)
The invention discloses a production method of 2-(4-bromomethyl phenyl)propionic acid. An adopted ionic liquid catalyst can be recycled and used, no molten aluminum trichloride is generated, a material does not need to be washed for multiple times, only layered extraction needs to be conducted, then a required product can be obtained, aluminum trichloride and triethanolamine salt ionic liquid is used, thus environmentally friendliness is achieved, the cost is also saved, and that is, an original cumbersome process is simplified. An original bromination reaction in a glass kettle is changed toa cooling glass pipeline circulation-type bromination reaction in the kettle, through the glass pipeline type reaction, the contact area of the material and light is increased, through circulation, the situation that the material is gathered on the illumination surface, and consequently light illumination is affected is avoided, thus the reaction efficiency is higher, the reaction time is shortened, the occurrence of a side reaction is controlled, and the product purity is higher.
Preparation method of p-bromomethyl isophenylpropionic acid
-
Paragraph 0014; 0015; 0044; 0049; 0050; 0051; 0056; 0057, (2020/08/09)
The invention belongs to the field of synthesis of drug intermediates, and particularly relates to a preparation method of p-bromomethyl isophenylpropionic acid, which comprises the following steps: A, synthesis of alpha-methyl benzyl chloride: carrying out addition reaction on styrene serving as a raw material and hydrogen chloride gas in an organic solvent to generate alpha-methyl benzyl chloride, B, synthesis of 2-phenylpropionic acid: preparing alpha-methyl benzyl chloride into a Grignard solution through a Grignard reaction, the Grignard solution and carbon dioxide gas are subjected to acarboxylation reaction to generate a carboxylation solution, and the carboxylation solution is hydrolyzed to obtain 2-phenylpropionic acid, and C, synthesis of p-bromomethyl isophenylpropionic acid: carrying out bromomethylation reaction of 2-phenylpropionic acid, hydrobromic acid and polyformaldehyde so that p-bromomethyl isophenylpropionic acid is generated. The preparation method of p-bromomethyl isophenylpropionic acid provided by the invention has the advantages of cheap and accessible raw materials and simple technique, and is suitable for industrial production.
Novel synthesizing method of 2-(4-bromomethyl)phenylpropionic acid
-
, (2019/06/08)
The invention belongs to the field of preparation of intermediates in chemical engineering, and particularly relates to a novel synthesizing method of 2-(4-bromomethyl)phenylpropionic acid. The novelsynthesizing method comprises the following steps of using 4-methyl acetophenone as the raw material; performing reduction, chlorinating and cyaniding, so as to obtain 2-(4-methyl)phenylpropionitrile;hydrolyzing, and brominating, so as to obtain the 2-(4-bromomethyl)phenylpropionic acid. The novel synthesizing method has the advantages that the yield rate is increased, and the cost of raw material is low; the novel synthesizing method is suitable for industrialized production.
Liquid-phase circulation preparation method for 2-(4-bromomethylphenyl)propionic acid
-
Paragraph 0063-0075; 0077; 0089-0095; 0097-0099; 0101-0103, (2019/01/22)
The invention discloses a liquid-phase circulation preparation method for 2-(4-bromomethylphenyl)propionic acid. The liquid-phase circulation preparation method comprises the following steps: feedinghydrobromic acid, paraformaldehyde, 2-phenylpropionic acid, a solvent and a Lewis acid catalyst in a bromoethylation reactor as reaction materials; adding water into a hydrogen bromide gas generator,adding phosphorus tribromide drop by drop, and allowing generated hydrogen bromide gas to pass through a buffer device and then to enter the bromoethylation reactor; heating the bromoethylation reactor to 60-80 DEG C, conveying a liquid phase in the reactor to a spray thrower through a liquid-phase circulation pump, spraying the liquid phase into a filler by the spray thrower so as to allow the liquid phase and the hydrogen bromide gas to fully contact in the filler, and carrying out reaction-absorption to achieve liquid-phase circulation; and after a reaction is completed, subjecting a reaction liquid in the bromoethylation reactor to post-treatment so as to obtain 2-(4-bromomethylphenyl)propionic acid. The method has the advantages of small amount of waste gas, waste water and industrialresidues, low cost and environment friendliness when applied to preparation of 2-(4-bromomethylphenyl)propionic acid.
Gas-phase circulation preparation method for 2-(4-bromomethylphenyl)propionic acid
-
Page/Page column 8-12, (2019/01/24)
The invention discloses a gas-phase circulation preparation method for 2-(4-bromomethylphenyl)propionic acid. The gas-phase circulation preparation method comprises the following steps: feeding hydrobromic acid, paraformaldehyde and 2-phenylpropionic acid in a bromoethylation reactor and adding a solvent and a Lewis acid catalyst as reaction materials; adding water into a hydrogen bromide gas generator, adding phosphorus tribromide drop by drop, and allowing generated hydrogen bromide gas to enter a buffer device; after heating of the bromoethylation reactor, allowing a gas phase of the reaction materials to enter a condenser for condensation, combining uncondensed gas with hydrogen bromide gas discharged from the buffer device, then allowing the obtained gas mixture to enter a gas circulation pump, and conveying the gas mixture to the bottom of the bromoethylation reactor by the gas circulation pump so as to realize gas-phase circulation; and after a reaction is completed, subjectinga reaction liquid in the bromoethylation reactor to post-treatment so as to obtain 2-(4-bromomethylphenyl)propionic acid. The method has the advantages of small amount of waste gas, waste water and industrial residues, low cost and environment friendliness when applied to preparation of 2-(4-bromomethylphenyl)propionic acid.
Synthetic method of 2-(4-bromomethyl)phenylpropionic acid
-
Paragraph 0024; 0025; 0026; 0027; 0028; 0029; 0030; 0031, (2018/03/26)
The invention provides a synthetic method of 2-(4-bromomethyl)phenylpropionic acid. The synthetic method comprises the following steps: (1) by taking 2-phenylpropionic acid as a raw material, bromineionic liquid as a reaction solvent, and formaldehyde and hydrogen bromide as bromoethylation reagents, enabling a reaction at a certain temperature for a certain period of time; (2) extracting 2-(4-bromomethyl)phenylpropionic acid from the product of the step (1) by use of an organic solvent, washing the extract containing 2-(4-bromomethyl)phenylpropionic acid with water, performing concentrationto obtain a 2-(4-bromomethyl)phenylpropionic acid crude product, and recrystallizing the crude product by a solvent to obtain a 2-(4-bromomethyl)phenylpropionic acid quality product; and (3) removingmost water and the organic solvent in bromine ionic liquid after extraction.
Method for preparing loxoprofen sodium
-
, (2017/07/12)
The invention relates to the technical field of organic synthesis, in particular to a method for preparing loxoprofen sodium. The invention provides a compound with the structure shown in formula 5 and a preparation method and application of the compound, (the formula is defined in the description). The loxoprofen sodium obtained according to the scheme is high in purity, high in industrialized operation, and good in application prospect.
Preparation method of 2-(4-bromomethyl)phenyl propionic acid
-
, (2018/01/11)
The invention discloses a preparation method of 2-(4-bromomethyl)phenyl propionic acid. The preparation method includes the steps of: performing a reaction to a compound (I) (4-methylstyrene) with hydrogen halide to prepare a compound (II), performing a Grignard reaction and a carboxylation reaction to the compound (II) to obtain a compound (IV), and performing a bromination reaction to obtain a compound (V) (2-(4-bromomethyl)phenyl propionic acid), wherein a byproduct compound (VI) is subjected to a debromination reaction to obtain the compound (V) (2-(4-bromomethyl)phenyl propionic acid). The method is low in cost, has simple operations, is high in yield, is environment-friendly, and is suitable for industrial production.
Pipelization preparation method and device for 2-(4-bromomethylphenyl)propionic acid
-
Paragraph 0031-0048; 0049; 0050; 0051-0054, (2018/04/01)
The invention discloses a pipelization preparation method and device for 2-(4-bromomethylphenyl)propionic acid and belongs to the technical field of pharmaceuticals. On one hand, the invention provides the pipelization preparation device for 2-(4-bromomethylphenyl)propionic acid, and the device comprises two tubular photoreactors internally provided with light sources, two mixers, three storage devices, three metering pumps, two water circulating pumps, two water bath kettles and one crystallization kettle. On the other hand, the invention provides the method for preparing 2-(4-bromomethylphenyl)propionic acid by using the device, and the method is simple in operation, mild in reaction condition, simple in aftertreatment, low in waste gas, waste water and waste residue production, high in atom utilization ratio, low in cost and high in economic benefit and is a green and environment-friendly process suitable for industrial production.
