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

Process for preparing 4-fluorobenzylamine with nano nickel as catalyst

A technology of p-fluorobenzylamine and catalyst, which is applied in the field of preparation of p-fluorobenzylamine, can solve the problems of long reaction time, high reaction temperature and low product purity, and achieve the effects of fast reaction speed, simple operation and advanced technology

Inactive Publication Date: 2005-12-07
张炳庚
View PDF0 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing preparation method of p-fluorobenzylamine is to make p-fluorobenzaldehyde hydrogenation by p-fluorobenzaldehyde, methyl alcohol, liquefied ammonia as catalyzer with Raney nickel, the production technology requirement of this method is high, and used pressure is big (4- 5Mpa), reaction temperature is high (above 170 ℃), and hydrogen utilization rate is little, and reaction time is long (about 5 hours), and cost is high, and product yield is low (below 80%), and catalyst consumption is big (about p-fluorobenzaldehyde consumption more than 5%), product purity is low (below 97%)

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
  • Process for preparing 4-fluorobenzylamine with nano nickel as catalyst
  • Process for preparing 4-fluorobenzylamine with nano nickel as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation steps of the present invention are as follows:

[0015] Step 1: be that 99% p-fluorobenzaldehyde 300Kg, anhydrous methanol 150Kg, nano-nickel catalyst 0.6Kg drop into 1000L autoclave, pass into liquid ammonia 30Kg, its feed intake weight ratio is: p-fluorobenzaldehyde: methyl alcohol: Liquid ammonia=1: 0.5: 0.10; the consumption of nano-nickel catalyst is 0.2% of the consumption of p-fluorobenzaldehyde.

[0016] Step 2: Heat up the temperature to about 70°C with steam under the stirring state, and then introduce pressure hydrogen into the reaction kettle, the pressure is 1Mpa-3Mpa;

[0017] Step 3: make the reaction fully until no hydrogen is absorbed, the reaction time is about 4 hours, and after the reaction stops, it is incubated for about 1 hour. After the reaction mixture is cooled, it is pressed into the fine-setting kettle, and the nano-nickel catalyst is separated by the fine-setting method to obtain crude p-fluorobenzylamine containing methanol...

Embodiment 2

[0020] Step 1: be that 99% p-fluorobenzaldehyde 300Kg, anhydrous methanol 300Kg, nano-nickel catalyst 1.8Kg drop into 1000L autoclave, pass into liquefied ammonia 45Kg, its feed intake weight ratio is: p-fluorobenzaldehyde: methyl alcohol: Liquid ammonia=1:1:0.15; the consumption of nano-nickel catalyst is 0.6% of the consumption of p-fluorobenzaldehyde.

[0021] Step 2: Stir and heat up to about 100°C, then feed hydrogen under pressure into the reactor, the pressure is 1Mpa-3Mpa;

[0022] Step 3: Make the reaction fully until no hydrogen is absorbed. The reaction time is about 3 hours. After the reaction stops, it is kept warm for 1 hour. The crude product of p-fluorobenzylamine in methanol;

[0023] Step 4: put the crude product of p-fluorobenzylamine obtained in step 3 into a rectification kettle for rectification, deamination before 80°C and recover methanol, dehydrate at 100°C, collect p-fluorobenzylamine at 186°C-190°C, and obtain a content greater than 99% The product...

Embodiment 3

[0025] Step 1: be that 99% p-fluorobenzaldehyde 300Kg, anhydrous methanol 600Kg, nano-nickel catalyst 3Kg drop into 1000L autoclave, pass into liquid ammonia 60Kg, its feed intake weight ratio is: p-fluorobenzaldehyde: methyl alcohol: liquid Ammonia=1:2:0.2; the consumption of nano-nickel catalyst is 1% of the consumption of p-fluorobenzaldehyde.

[0026] Step 2: Stir and heat up to 120°C, then feed hydrogen under pressure into the reactor, the pressure is 1Mpa-3Mpa;

[0027] Step 3: Make the reaction fully until no hydrogen is absorbed. The reaction time is about 1 hour. After the reaction is stopped, it is incubated for about 1 hour. After the reaction mixture is cooled, it is pressed into the fine-setting kettle, and the nano-nickel catalyst is separated by the fine-setting method to obtain crude p-fluorobenzylamine containing methanol;

[0028] Step 4: put the crude product of p-fluorobenzylamine obtained in step 3 into a rectification kettle for rectification, deaminatio...

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 process for preparing 4-fluorobenzylamine with nano nickel as catalyst, which employs 4-fluorobenzaldehyde, hydrogen, absolute methanol, liquid ammonia as raw material. Test results show that, under the same reaction conditions, the process of the present invention can realize an average yield of above 95%, and a purity above 99%.

Description

Technical field: [0001] The invention relates to a preparation method of p-fluorobenzylamine. Background technique: [0002] p-Fluorobenzylamine is a pharmaceutical intermediate and a raw material for organic synthesis. The existing preparation method of p-fluorobenzylamine is to make p-fluorobenzaldehyde hydrogenation by p-fluorobenzaldehyde, methyl alcohol, liquefied ammonia as catalyzer with Raney nickel, the production technology requirement of this method is high, and used pressure is big (4- 5Mpa), reaction temperature is high (above 170 ℃), and hydrogen utilization rate is little, and reaction time is long (about 5 hours), and cost is high, and product yield is low (below 80%), and catalyst consumption is big (about p-fluorobenzaldehyde consumption More than 5% of), product purity is low (below 97%). Invention content: [0003] The object of the present invention is to provide a kind of method that takes nano-nickel as catalyst to prepare p-fluorobenzylamine. [...

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): C07C211/29
Inventor 张炳庚
Owner 张炳庚
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