Preparation method of 4-cylopropylamine ethyl butyrate
The technology of ethyl cyclopropylaminobutyrate and ethyl bromobutyrate is applied to the preparation of ethyl 4-cyclopropylaminobutyrate and the field of pharmaceutical intermediates, and can solve the problems of difficult recovery of reaction solvent, low yield and the like, Achieve the effect of easy recovery of raw materials, high molar yield and cost reduction
Inactive Publication Date: 2015-11-04
上海博康睿玉贸易发展有限公司
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Problems solved by technology
[0005] For the above-mentioned technical problems in the prior art, the invention provides a kind of preparation method of ethyl 4-cyclopropylamino butyrate, the preparation method of described this ethyl 4-cyclopropylamino butyrate solves existing The preparation method in the technology has low yield and the technical problem that the reaction solvent is difficult to recover
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Embodiment 1
[0015] Put 34.4g of cyclopropylamine and 176g of dimethyl sulfoxide into a 500ml four-necked flask in turn, stir, add 40g of ethyl 4-bromobutyrate dropwise at 15-20°C, drop it in 4 hours, keep stirring for 2 hours, the raw material After the reaction, take samples and send them to GC (central control 1). After the reaction, add 350ml of water and 200ml of ether to the reaction, extract and separate layers, separate the ether layer, extract the water layer with 200ml of ether once more, combine the ether layers, and re-extract the ether layers. Extract once with 350ml of water, and dry the ether layer with anhydrous sodium sulfate. After spin-drying, the net weight of the liquid is 28.6g. Gas phase analysis (center control 2) put the liquid into another 500ml four-necked flask, and add 350ml of methyl tert-butyl Base ether, stirring, below 25°C, pass hydrogen chloride gas (60ml concentrated sulfuric acid is added dropwise to 120ml concentrated hydrochloric acid, wash the gas bot...
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The invention relates to a preparation method of 4-cylopropylamine ethyl butyrate. The preparation method comprises the steps: in a reaction container, firstly adding cylopropylamine and dimethyl sulfoxide, stirring, and dropwise adding ethyl 4-bromobutyrate at the temperature of 15-20 DEG C; after dropwise adding is finished, carrying out heat-preservation stirring, after the reaction is finished, adding water and ethyl ether, extracting and layering, drying an ether layer, and spin-drying; adding the substance into another reaction container, adding methyl tert-butyl ether, dissolving, stirring, and introducing hydrogen chloride gas; after introduction of hydrogen chloride is finished, carrying out heat-preservation stirring, and filtering, to obtain a white solid; putting the white solid into another reaction container, adding ethyl acetate, carrying out heating reflux, then cooling, and filtering to obtain a solid; and again adding the solid into another reaction container, adjusting the pH of the solution to 8-10 with an alkali solution, adding dichloromethane and extracting, drying a dichloromethane layer, and spin-drying to obtain 4-cylopropylamine ethyl butyrate. The yield is high, the raw materials are all relatively easy to recycle, the production cost is reduced, maneuverability is high, and the preparation method has industrial application prospects.
Description
technical field [0001] The invention belongs to the field of organic chemistry, in particular to a pharmaceutical intermediate, specifically a preparation method of ethyl 4-cyclopropylaminobutyrate. Background technique [0002] Ethyl 4-cyclopropylaminobutyrate is a pharmaceutical intermediate, which can be used as a compound for the synthesis of pharmaceuticals or as an intermediate. [0003] In the prior art, cyclopropylamine is used directly as a solvent, and the reaction is complete within 3 hours, but the main content is only 70%, and cyclopropylamine has a low boiling point and is difficult to recover, and the price is relatively expensive. There are also ethanol, diethyl ether, methyl tert-butyl ether, triethylamine, and DMF as solvents, but the main content of the reaction product is also low, and there is no industrial application prospect. [0004] The M-phase kinesin Eg5 is important as a target molecule for novel M-phase-acting agents, and its inhibitors are con...
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IPC IPC(8): C07C229/14C07C227/08
Inventor 傅志伟贺宝元潘新刚牟立娟邵严亮
Owner 上海博康睿玉贸易发展有限公司