Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for continuously synthesizing homopiperazine

A technology of homopiperazine and mixed gas, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Problems such as recycling and regeneration, synthetic routes cannot be reproduced repeatedly, etc., to achieve the effects of stable activity, good catalytic effect and long service life

Pending Publication Date: 2022-05-13
上海巽田科技股份有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This method solves the problem that the protective reagent cannot be recycled and regenerated, avoids highly corrosive concentrated sulfuric acid and hydrofluoric acid, and improves environmental protection and safety. Discontinuous batch production cannot fully meet the needs of industrial production
[0010] (2) Using N-(2-cyanoethyl)ethylenediamine as a raw material: In 1961, Poppludoef et al. used N-(2-cyanoethyl)ethylenediamine as a raw material and Gedler G-49A as a catalyst. Homopiperazine was obtained by hydrogenation cyclization, but the yield was only 32.4% (J.Org.Chem., 1961, 26(1):131-134)
[0024] However, the synthetic route reported in the literature does not seem to be able to be reproduced repeatedly, and its effectiveness cannot be demonstrated

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for continuously synthesizing homopiperazine
  • Method for continuously synthesizing homopiperazine
  • Method for continuously synthesizing homopiperazine

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0083] The preparation method of the catalyst may be a precipitation method, an impregnation method, a blending method, a sol-gel method; preferably a precipitation method and an impregnation method.

[0084]Preferably, the preparation method of the catalyst is carried out as follows: the catalyst active component precursor metal hydrochloride or nitrate (selected from ruthenium (Ru), platinum (Pt), rhodium (Rh)) or gold (Au) Sulfate or nitrate is dissolved in water or alcohol to form a solution, and the active component is deposited and precipitated by forward dripping with lye at 20-80°C. When the pH of the system reaches 2-5, the carrier powder is added, and then the second Second active component metal solution (such as ammonium perrhenate, manganese acetate, etc.), the concentration of the second active component solution is controlled at 0.05-0.5mol / L, continue to titrate the lye until the pH of the system reaches 12-13, fully stir beating and aging 3-12 hours, after agi...

preparation Embodiment 1

[0089] Preparation Example 1: 5wt%Ru-1wt%ReOx / TiO 2 Preparation of:

[0090] Weigh 100g of TiO2 (P25, Evonik Degussa, Germany) and vacuum degass at 150°C for 12h before use. 13.5g of ruthenium trichloride hydrate (Ru content 37.5%, Sinopharm Chemical Reagent Co., Ltd.) was dissolved in 50ml of water to form a catalyst precursor solution, the catalyst precursor solution was heated to 40°C, and 10% ammonia water was added dropwise forward to make When the pH of the system reaches 2.5, put in the catalyst carrier powder, stir and impregnate for 3 hours; dissolve 1.5g of ammonium perrhenate (purchased from Beijing Bailingwei Technology Co., Ltd.) in 20ml of water, add the above slurry, and continue to titrate 10% ammonia water until the pH of the system reaches 12. Fully stir and beating and aging for 12 hours. After aging, filter and wash the slurry until the filtrate becomes neutral. After adding the forming auxiliary scallop powder, the slurry is extruded into 3mm round bars o...

preparation Embodiment 2

[0091] Preparation Example 2: 5wt%Ru-10wt%ReOx / TiO 2 preparation of

[0092] The preparation method is the same as that of Catalyst Preparation Example 1, except that the amount of ammonium perrhenate is increased to 15 g. The catalyst prepared according to this method is labeled as 5wt%Ru-10wt%ReOx / TiO 2 .

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for one-step synthesis of homopiperazine through catalysis, and the method comprises the following steps: mixing an N-(beta-hydroxy)-1, 3-propane diamine solution with hydrogen or a mixed gas of hydrogen and ammonia gas, introducing the mixture into a continuous reactor filled with a catalyst, carrying out a reaction, collecting a reaction product, and separating to obtain a homopiperazine product. Compared with the prior art, the method has the advantages that N-(beta-hydroxyl)-1, 3-propane diamine is used as a raw material, the heterogeneous noble catalyst is adopted, the process is simple, safe and reliable, the service life of the catalyst is long, the process is stable, and the method is suitable for industrial continuous production; compared with the existing reported Cu-based catalyst, the catalyst has the advantages of obvious effect and long service life. The catalyst has the advantages of easily available raw materials, simple preparation, stable activity, long service life and good catalytic effect.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method capable of continuously synthesizing homopiperazine. Background technique [0002] Homopiperazine, also known as 1,4-diazepane or 1,4-diaminocyclooctane, is an aza seven-membered ring compound. Homopiperazine is an important intermediate in organic synthesis. The dinitrogen atom contained in it can react with many organic compounds. It is widely used in the structural modification and transformation of chemical drugs. It is an important link between the chemical industry and the pharmaceutical field. product. Homopiperazine and its derivatives are not only widely used in fine chemical fields such as antioxidants, foaming agents, emulsifiers, and surfactants, but also play an indispensable role in the fields of medicine and pesticides. Homopiperazine can be used to synthesize fasudil hydrochloride, homopiperazine hydrochloride, cyclizine, carbamaze...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D243/08B01J23/656
CPCC07D243/08B01J23/6567
Inventor 牟新东王喜成许宏金
Owner 上海巽田科技股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com