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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 high cost, and achieve the effects of fast reaction speed, simple operation and reduced cost

Inactive Publication Date: 2009-01-21
张炳庚
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  • 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

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

Examples

Experimental program
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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, deaminat...

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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

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/29C07C209/26
Inventor 张炳庚
Owner 张炳庚
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