Method for producing monoacetylated homopiperazine

A technology for monoacetyl homopiperazine and homopiperazine, which is applied in the field of producing monoacetyl homopiperazine, can solve problems such as being difficult to realize industrialization, and achieve the effects of easy operation, high yield and mild reaction conditions

Inactive Publication Date: 2010-06-16
大连凯飞精细化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0019] In the presence of Ru3(CO)12 and Bu3P, ethylene glycol and ethylenediamine undergo cyclization and condensation reactions, and the

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  • Method for producing monoacetylated homopiperazine

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Example Embodiment

[0031] Example 1

[0032] Intermediate product of the first step 1: At 10-20℃, add ethylenediamine (70g, 1.17mol) in water (163ml) to a 2L four-neck flask, stir, and add sodium hydroxide to the reaction system Aqueous solution (114g, 2.85mol, 746ml of water), when the temperature is lowered by 10-20°C, add p-toluenesulfonyl chloride (496.6g, 2.6mol) in batches, after the addition, stir for 5-6 hours. Filter for 1-2 days (although the reaction solution is viscous and difficult to filter, but try to filter because there are inorganic salts in the solution), the filter cake is slurried with ethanol at 60℃, stirred for 30 minutes, and when the temperature is cooled to room temperature, filter again. The cake was washed with ethanol and dried to constant weight by infrared to obtain a white solid intermediate product (318 g) with a yield of 72.6%.

[0033] Intermediate product 2: Intermediate product 1 (36.8g, 0.1mol), tetrabutylammonium bromide (8g, 0.025mol), toluene (400ml), 5% sodi...

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Abstract

The invention discloses a method for preparing monoacetylated homopiperazine. Corresponding homopiperazine bromate is prepared and neutralized under the alkaling condition by taking water as solvent; at about 0 DEG C, acetic anhydride is adopted for monoacetylated reaction. The invention starts from simple raw material to design and combine homopiperazine bromate which has reasonable route and is prepared by ethene diamine via sulfonylation, ring formation and removing sulfonyl; the homopiperazine bromate is alkalified and monoacetylated to finally generate the target product. The invention has moderate reaction condition, quick reaction, simple technology and easy operation, is suitable for industrial large-scale production, has high yield and high purity and satisfies the application requirements of pharmaceuticals industry and the like.

Description

Technical field: [0001] The present invention relates to a method for preparing organic compounds, especially a method for preparing homopiperazine. Background technique: [0002] Seven-membered heterocycles are multilateral rings. Most of their intermediates have strong biological activity and medicinal value. Nitrogen-containing heterocyclic compound homopiperazine is an important intermediate for drug synthesis. The double nitrogen atom contained in it can interact with many organic compounds. Reaction, especially in the structural modification and transformation of chemical drugs, plays an extremely important role. Homopiperazine and its homopiperazine derivatives have become important drug intermediates with great potential for sedation, antipsychotic, anti-inflammatory and anti-neuropathy. They are important products connecting the chemical industry and the pharmaceutical industry. They are widely used in medicine, Pesticides, surfactants, energetic materials and other fie...

Claims

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Application Information

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IPC IPC(8): C07D243/08
Inventor 张殿举王乃伟秦学孔
Owner 大连凯飞精细化工有限公司
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