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

A kind of method for high-selectivity oxidation of benzylamine green synthesis of n-benzyl butylamine

A technology of benzylamine oxide and synthesis method, which is applied in chemical instruments and methods, imino compound preparation, metal/metal oxide/metal hydroxide catalyst, etc., and can solve high reaction temperature, weak visible light response, and photocatalytic activity Low-level problems, to achieve the effect of low energy consumption

Active Publication Date: 2019-03-29
HUNAN UNIV
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some defects in the existing oxidation method: higher reaction temperature, longer reaction time, a large amount of organic solvent used in the reaction or post-treatment
However, these photocatalysts have disadvantages such as low photocatalytic activity and weak response to visible light.

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
  • A kind of method for high-selectivity oxidation of benzylamine green synthesis of n-benzyl butylamine
  • A kind of method for high-selectivity oxidation of benzylamine green synthesis of n-benzyl butylamine
  • A kind of method for high-selectivity oxidation of benzylamine green synthesis of n-benzyl butylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The present invention prepares the photocatalyst with the different molar ratios of chromium tungstate and bismuth tungstate in the cadmium tungstate-bismuth tungstate composite photocatalyst:

[0023] Preparation of cadmium tungstate: Dissolve 1.234g cadmium nitrate in 40ml deionized water and mix with 0.240g ethylenediamine solution, stir well to form solution A; dissolve sodium tungstate in 40ml water to obtain solution B; mix and stir AB for 10min , to obtain solution C; then the obtained solution C was crystallized at 180° C. for 20 hours. The crystallization solution is separated by cooling and filtration, washed three times with deionized water and once with absolute ethanol, and dried at 80°C for 6 hours to obtain cadmium tungstate;

[0024] Preparation of composite material: Dissolve 0.041g of sodium tungstate in 10ml of ethylene glycol solution, stir well to form solution D; dissolve 0.121g of bismuth nitrate in 10ml of ethylene glycol solution, stir well to f...

Embodiment 2～5

[0028] For cadmium tungstate and bismuth tungstate composite photocatalysts with different molar ratios, the operation steps are similar to those in Example 1, only the amount of sodium tungstate and bismuth nitrate in the composite material is changed, and the rest of the conditions are unchanged, and the sample number is Cat 2, Cat 3, Cat 4, Cat 5. See Table 1 for the composite catalyst conditions and reaction results prepared in Examples 1-5.

[0029] Table 1 Preparation conditions and reaction results of composite photocatalysts with different molar ratios

[0030]

[0031] It is found from Table 1 that the ratio of Cat 4 cadmium tungstate-bismuth tungstate makes the conversion rate of benzylamine 38.7%, the selectivity of N-benzylbutylamine is greater than 99%, and has the best photocatalytic effect.

Embodiment 6～10

[0033] According to the step 4 of the embodiment in which the molar ratio of chromium tungstate and bismuth tungstate in the reaction mixture has the best effect is 1:7.5, the remaining conditions remain unchanged, and the crystallization temperature prepared by the composite photocatalyst is changed, respectively using 100°C, 120°C, After crystallization at 140°C, 180°C, and 200°C for 24 hours, the samples were respectively coded as T 1, T 2, T 3, T 4, and T 5, and the rest of the operation steps were similar to those in Example 4. See Table 2 for the composite catalyst conditions and reaction results prepared in Examples 6-10.

[0034] Table 2 The molar ratio of chromium tungstate and bismuth tungstate is 1:7.5 and different crystallization temperature conditions and reaction results

[0035]

[0036]

[0037] It is found from Table 2 that different benzylamine conversion rates are obtained at different crystallization temperatures, and the temperature is compared with...

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 provides a method for green synthesis of N-benzylbutylamine by oxidizing benzylamine with high selectivity. The method includes: dissolving cadmium tungstate and bismuth tungstate in an alcohol solution, stirring and mixing evenly; crystallizing the mixed solution, and then performing cooling, filtration, separation, drying and other steps to prepare cadmium tungstate-bismuth tungstate. Composite photocatalyst: Take the cadmium tungstate-bismuth tungstate composite photocatalyst and disperse it in benzylamine, add oxygen and light to obtain N-benzylbutylamine. The present invention can improve the conversion rate of benzylamine by controlling the proportion of the catalyst, and the selectivity of the prepared N-benzylbutylamine is greater than 99%. The invention has the characteristics of green, solvent-free, high efficiency, low energy consumption and simple synthesis process.

Description

【Technical field】 [0001] The invention relates to the field of photocatalytic oxidation, in particular to a method for green synthesis of N-benzylbutylamine by highly selective oxidation of benzylamine. 【Background technique】 [0002] Imines are important intermediates in organic synthesis and have important applications in the field of biomedicine. Due to the electrophilic double bond, imines can undergo important reactions with other reagents. As an important chemical product that can be used to synthesize biologically active natural products and drug candidates, N-benzylbutylamine can undergo addition reactions with esters, acid chlorides, enones, etc. to generate β-lactams, and β- The wide application of lactam antibiotics makes the oxidation of benzylamine to N-benzylbutylamine important. The traditional synthesis method adopts the condensation of primary amines and aldehydes and ketones. This method requires a heating dehydration device, the operation is troublesome...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/02C07C251/24B01J23/31
CPCC07C249/02B01J23/31B01J35/39C07C251/24
Inventor 尹双凤陈鹏陈浪蒋旭曾誉刘娜
Owner HUNAN UNIV
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