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Preparation method of methyl ethylamine

A technology for methylethylamine and formylethylamide, which is applied in the field of preparation of methylethylamine, can solve problems such as being unsuitable for industrial production, and achieve the effects of simple and easy-to-obtain starting materials, stable and controllable quality, and simple and easy reaction operation.

Inactive Publication Date: 2007-10-31
HAINAN SHENGKE LIFE SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Wherein by Shiff base preparation quaternary ammonium salt step, used reagent CH 3 I boiling point is 42~43 ℃, and this method reaction temperature needs to reach more than 100 ℃, so reaction vessel needs sealing high pressure, is not suitable for industrialized production

Method used

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  • Preparation method of methyl ethylamine
  • Preparation method of methyl ethylamine
  • Preparation method of methyl ethylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment one: the preparation of formyl ethylamide

[0021] Add 7.5 L of methyl formate to the reaction kettle and cool to about 0°C. Maintaining less than 10°C, add 650g of ethylamine dropwise. After the dropwise addition was completed, the mixture was slowly heated to reflux for 4 hours. After the reaction was completed, the reaction solution was concentrated. Add toluene and concentrate under reduced pressure 250 mL x 3 times to obtain light yellow oil. equimolar yield.

Embodiment 2

[0022] Embodiment two: the preparation of formyl ethylamide

[0023] 15 L of ethyl formate was added to the reaction kettle. Maintain a solution of 1300 g of ethylamine in 1.5 L of ethanol dropwise at less than 10 ° C. After the dropwise addition was completed, the reaction was carried out at room temperature for 20 hours. After the reaction was completed, the reaction solution was concentrated. Add toluene and concentrate under reduced pressure 500 mL x 3 times to obtain light yellow oil with equimolar yield.

Embodiment 3

[0024] Embodiment three: the preparation of formyl ethylamide

[0025] Add 1.5 L of ethyl formate to the reaction kettle and cool to about 0°C. Maintain a solution of 1300 g of ethylamine in 1.5 L of ethanol dropwise at less than 10 ° C. After the dropwise addition was completed, the mixture was heated to reflux for 4 hours. After the reaction was completed, the reaction solution was concentrated. Add toluene and concentrate under reduced pressure 500 mL x 3 times to obtain light yellow oil with equimolar yield.

[0026] Embodiment two: the preparation of methylethylamine

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Abstract

The invention discloses a preparing method of nail ethanol, which is characterized by the following: the nail ethanol is a critical raw material of the medicine to cure Alzheimer's disease (AD). This invention possesses lower cost, simple operation, higher receiving ratio and stable quality, which can be fit for industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of methylethylamine. The derivative can be used to prepare the anti-moderate Alzheimer's disease (AD) drug rivastigmine. Background technique [0002] Rivastigmine is used for the treatment of moderate Alzheimer's disease (AD), and is a carbamate acetylcholinesterase inhibitor. It has the following chemical structure: [0003] [0004] In the published literature EP0193926, the classic synthetic route of rivastigmine is as follows: [0005] [0006] Wherein methylethylamine is the key raw material of synthesizing rivastigmine, according to literature data OrgnicSynthesis.Coll.Vol 5:758 the synthetic route of methylethylamine is as follows: [0007] [0008] Wherein by Shiff base preparation quaternary ammonium salt step, used reagent CH 3 I boiling point is 42~43 ℃, and this method reaction temperature needs to reach more than 100 ℃, so reaction vessel needs sealing high pressur...

Claims

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Application Information

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IPC IPC(8): C07C209/50C07C211/03
Inventor 康彦龙
Owner HAINAN SHENGKE LIFE SCI RES INST
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