Synthetic method of 5-(N-ethyl-N-2-ethylol amine)-2-amylamine

A technology of hydroxyethylamine and a synthesis method, which is applied in the synthesis field of 5--2-pentylamine, can solve the problems of low purity of target product, low total yield and the like, and achieves easy industrial production, high conversion rate of raw materials, Avoid the effect of separation operations

Inactive Publication Date: 2015-07-29
WUHAN RUIKAIXING SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, because there is no protective ketone group, 5-chloro-2-pentanone is prone to side reactions under reaction conditions to generate cyclopropylmethyl ketone, so that the purity of the target product is not high, and the overall yield is not high

Method used

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  • Synthetic method of 5-(N-ethyl-N-2-ethylol amine)-2-amylamine
  • Synthetic method of 5-(N-ethyl-N-2-ethylol amine)-2-amylamine
  • Synthetic method of 5-(N-ethyl-N-2-ethylol amine)-2-amylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of synthetic method of 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine, its step is as follows:

[0027] (1) Preparation of catalyst: Disperse and dissolve 0.5g or 20 or 40 or 60 or 80 or 100g of cobalt nitrate into 100ml or 1 or 2L of ethanol, then add 5g or 50 or 200 or 500 or 1000 or 1500 or 2000g of oxidized Magnesium nanopowder, stirred and ultrasonicated at 40 or 45 or 50 or 59 Hz for 10 or 30 or 60 minutes, evaporated the ethanol solvent to dryness, and vacuum dried at 80 or 90 or 100 or 110 or 120°C for 1 or 3 or 5 Or 10 hours, and finally grind into a fine powder with a particle size of 0.5-2 microns to obtain 5-chloro-2-pentanone and N-ethylethanolamine to directly react to prepare 5-(N-ethyl-N-2-hydroxyethyl Catalyst for the reaction of amine)-2-pentanone.

[0028] (2) Add 1.0 or 1.3 or 1.5L of xylene, 320g or 325 or 330g of 5-chloro-2-pentanone and 470 or 480 or 490g of N-ethylethanolamine in turn in the reaction flask, start stirring, add 1.5 Or 3 ...

Embodiment 2

[0031] A kind of synthetic method of 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine, its step is as follows:

[0032] (1) Preparation of catalyst: Disperse and dissolve 0.5g or 25 or 45 or 65 or 85 or 100g of nickel nitrate into 100ml or 1 or 2L of ethanol, then add 5g or 60 or 220 or 600 or 1100 or 1600 or 2000g of oxidized Magnesium nanopowder, stirred and ultrasonicated at 40 or 44 or 51 or 59 Hz for 10 or 25 or 35 or 60 minutes, evaporated the ethanol solvent, and vacuum dried at 80 or 93 or 101 or 110 or 120°C for 1 or 3 Or 5 or 10 hours, and finally grind into a fine powder with a particle size of 0.5-2 microns to obtain 5-chloro-2-pentanone and N-ethylethanolamine to directly react to prepare 5-(N-ethyl-N-2- Catalyst for the reaction of hydroxyethylamine)-2-pentanone.

[0033] (2), sequentially add 1.0 or 1.2 or 1.5L xylene, 320 or 326 or 330g 5-chloro-2-pentanone and 470 or 482 or 490g N-ethylethanolamine in the reaction flask, start stirring, add 1.5 Or 4 or 6 or 9...

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Abstract

The invention discloses a synthetic method of 5-(N-ethyl-N-2-ethylol amine)-2-amylamine. The method comprises the following steps: (1) the preparation of a catalyst, to be specific, dispersing and dissolving nitrate into an organic solvent, adding oxide or nanopowder of carbonate into the organic solvent, after ultrasonic stirring, evaporating the organic solvent to dryness, carrying out vacuum drying and grinding the dried solvent into fine powder to obtain the catalyst; (2) adding xylene, 5-chlorine-2-pentanone and N-ethylethanolamine in a reaction flask in sequence, stirring the materials, adding the prepared catalyst, heating the flask to increase the temperature till reflux occurs, cooling the heated materials to room temperature, filtering the materials to obtain a filtrate, fractionating the filtrate to obtain 5-(N-ethyl-N-2-ethylol amine)-2-pentanone; (3) putting 5-(N-ethyl-N-2-ethylol amine)-2-pentanone in a hydrogenation flask, adding aminomethanol and raney nickel to perform reaction under hydrogen pressure; after the reaction, displacing the hydrogen and ammonia in the system with nitrogen, filtering the reaction liquid to obtain a filtrate, fractionating the filtrate to obtain 5-(N-ethyl-N-2-ethylol amine)-2-amylamine. The method is high in conversion rate, simple and convenient to operate, high in yield, low in cost, easy for industrial production, safe and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and more specifically relates to a synthesis method of 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine. Background technique [0002] The chemical name of racemic hydroxychloroquine is 7-chloro-4-[5-(N-ethyl-N-2-hydroxyethyl)-2-pentyl] aminoquinoline, and its structural formula is as follows: [0003] [0004] Racemic hydroxychloroquine sulfate is sold under the tradename Plaquenil RTM by the French company Sanofi Winthrop Industries. [0005] Hydroxychloroquine is prepared by the Fisher reaction of 4,7-dichloroquinoline and 5-(N-ethyl-N-2-hydroxyethylamine)-2-pentylamine, and the reaction formula is as follows: [0006] [0007] At present, hydroxychloroquine is clinically used as the first-line basic drug for the treatment of connective tissue disease lupus erythematosus (discoid, subacute cutaneous, systemic), and is also the first-line combined drug fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/14C07C213/08C07C213/02
Inventor 游海军刘昱宁凡郑卓于巧璐牛小斌李诚
Owner WUHAN RUIKAIXING SCI & TECH
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