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Novel preparation of fenspiride

A technology of fenspiride and a new method, applied in the field of preparation of fenspiride, can solve the problems of high cost, high price, unfavorable large-scale production, etc.

Inactive Publication Date: 2009-03-04
宁波保税区欣诺生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic route of the recent paper published by Synthetic Communications (24:10, 1483-1487) also uses highly toxic phosgene, and the price of other raw materials is also very expensive
The routes described in the above materials are all dangerous and expensive, which is not conducive to large-scale industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0007] Further describe the total synthesis of fenspiride below by the examples

[0008] Add 40L of methanol into a 100L reactor, feed 3 kg of 2-phenylethylamine and 20L of methyl acrylate under stirring, reflux for 10 hours, distill methanol off under reduced pressure to obtain double-tallow amine; add 20L of water to double-tallow amine, dissolve in 5L of concentrated hydrochloric acid, and reflux After 10 hours, cool down to 0°C, neutralize with 20% NaOH to pH = 12, and filter to obtain a light yellow powder product N-phenethyl-4-piperidone; add 5 L of ethyl 1-bromoacetate, and detect 1-bromoacetate by TLC Ethyl acetate reacted completely, added 10L of toluene-ether solution (1:2) dropwise, stirred for 2 hours, TLC detected that the reaction of N-phenethyl-4-piperidone was complete, filtered, and the powder was vacuum-dried at 60°C, and the product was dissolved in Add 10L of 85% hydrazine hydrate to 5L of toluene, react at room temperature for 5 days, distill under reduced...

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PUM

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Abstract

The invention discloses a new method for preparing fenspiride. The method is characterized in that methanol is adopted as a solvent; 1-phenylethylamine and methyl acrylate as raw material are subjected to the Michae addition and the Deckman condensation to synthesizing 1-phenyl-4-piperidone raw material with high efficiency; and 1-phenyl-4-piperidone is subjected to the Reformatsky reaction and the Curtius rearrangement to obtain the fenspiride product. The method is economic, safe and environment friendly, and is suitable for the industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a new method for preparing fenspiride. Background technique [0002] Background technology of the present invention is as follows: [0003] U.S. Patent (US3399192) uses 4-piperidone to generate 1-oxa-3,8-diazaspiro[4,5]dec-2-one, and then reacts with 1-chloro-2-phenylethane Produces fenspiride. In this synthetic route, 4-piperidone is first converted to 4-hydroxy-4-(1-nitro)methylpiperidine, and then the nitro group is reduced to an amino group by high-pressure hydrogenation using Niobium Niobium. The high-pressure hydrogenation reduction of Lei Niobium Nickel is a one-step flammable and explosive reaction. Lei Niobium Nickel is particularly prone to spontaneous fire and explosion during use. Industrial production is very dangerous and requires special explosion-proof workshops for production. Ring closure of 4-hydroxy-4-(1-amino)methylpiperidine and phosgene gene...

Claims

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Application Information

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IPC IPC(8): C07D498/10
Inventor 巫军
Owner 宁波保税区欣诺生物技术有限公司
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