Synthesizing method of 3-N,N-dimethylamino ethyl acrylate

Abstract

The invention discloses a method for preparing 3-N,N-dimethylamino ethyl acrylate from a transition metal carbonyl complex.The method comprises the steps that a specified amount of alkali metal alkoxide and alcohol-containing organic solvent or alkali metal and / or alkali metal hydride and the alcohol-containing organic solvent are taken as raw materials to react to generate an intermediate; a condensation reaction is performed for 4-10 h in a high-pressure reaction kettle by taking the intermediate, ethyl acetate and carbon monoxide gas or ethyl formate as raw material and taking a specified substance containing a transition metal element as a catalyst under the pressure of 2-5 MPa at the temperature of 50 DEG C-100 DEG C to generate a solution containing a specified alkali metal salt; the solution is added into an aqueous dimethylamine hydrochloride solution in batches to obtain 3-N,N-dimethylamino ethyl acrylate.According to the method, by adding the transition metal element, the raw material conversion rate and the product yield are increased, the product purity is improved, the economic benefit is increased, the raw materials are easy to obtain, the atom economy is good, and the raw material utilization rate is high; part of the original auxiliary materials are recycled and reused, and therefore discharge of three wastes is greatly reduced.

Description

technical field [0001] The invention relates to the field of medical materials, in particular to a synthesis method of ethyl 3-N,N-dimethylaminoacrylate. Background technique [0002] 3-N, N-ethyl dimethylaminoacrylate is a key intermediate in the synthesis of the main ring of quinolones, and has a large market demand. The structure of quinolones is as follows: [0003] [0004] Among them, the carboxyl group at the 3-position and the oxygen at the 4-position are essential groups, and a ring can be formed between the 1-position and the 8-position. Quinolones antibacterial drugs have the advantages of broad antibacterial spectrum, strong antibacterial activity, convenient administration, less toxic and side effects, and no cross-resistance with other antibiotics. Antimicrobials. [0005] The method of synthesizing the parent ring of quinolones mainly adopts intramolecular nucleophilic substitution reaction. Condensation reaction of acid chloride or substituted aromatic...

AI Technical Summary

Problems solved by technology

But method (9) uses " one pot method ", because dimethylamine is introduced in the reaction system prematurely, will cause impurity to increase, in order to obtain high-purity product, need to increase rectifying column tray number, improve equipment preparation, and Finally, it has an impact on the yield of high-purity products

The "one-pot method" includes two-step reactions at the same time, and the water produced in the second step reaction will inhibit the first step reaction, making the reaction incomplete and reducing the yield, so the purity and yield of the product are not ideal

Images