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

Preparation method of 3-methoxy-4-hydroxybenzylamine hydrochloride

A technology of hydroxybenzylamine hydrochloride and hydroxybenzaldehyde, which is applied in the field of chemical reagent synthesis technology, can solve the problems of low yield and high cost of the synthesis process, and achieve the effects of high product precision, reduced raw material costs, and simple operation

Inactive Publication Date: 2015-11-18
黄石市利福达医药化工有限公司
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the invention is to overcome the problems of low yield and high cost of the existing 3-methoxy-4-hydroxybenzylamine hydrochloride synthesis process

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
  • Preparation method of 3-methoxy-4-hydroxybenzylamine hydrochloride
  • Preparation method of 3-methoxy-4-hydroxybenzylamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The present embodiment provides a kind of preparation method of 3-methoxyl-4-hydroxybenzylamine hydrochloride specifically comprising the following steps:

[0022] 1) Dissolve 75g (0.49mol) of 3-methoxy-4-hydroxybenzaldehyde in 200g of anhydrous methanol in advance for later use.

[0023] 2) Pump the 3-methoxy-4-hydroxybenzaldehyde solution ready for use in step 1) into a 1L autoclave, start stirring, add 8g of Raney nickel catalyst, add 220g of anhydrous methanol, and close For all valves in the autoclave, first use vacuum to take away most of the air, and then introduce nitrogen until the pressure in the autoclave reaches 3kg / c㎡, and the pressure does not change. After confirming that the autoclave is well sealed, the nitrogen is discharged, and the operation is repeated 2 to 3 times. , replace all the air in the autoclave with nitrogen.

[0024] 3) Turn on the cooling water in the jacket of the autoclave, control the temperature in the autoclave to below 35°C, add 1...

Embodiment 2

[0033] The present embodiment provides a kind of preparation method of 3-methoxyl-4-hydroxybenzylamine hydrochloride specifically comprising the following steps:

[0034] 1) Dissolve 75g (0.49mol) of 3-methoxy-4-hydroxybenzaldehyde in 150g of anhydrous methanol in advance for later use.

[0035] 2) Pump the 3-methoxyl-4-hydroxybenzaldehyde solution ready for use in step 1) into a 1L autoclave, start stirring, add 6.25g of Raney nickel catalyst, and then add 220g of anhydrous methanol , close all the valves of the autoclave, first take away most of the air with vacuum, and then introduce nitrogen until the pressure in the autoclave reaches 3kg / c㎡, and there is no change in the pressure, confirm that the seal of the autoclave is intact, and then discharge the nitrogen, repeat the operation 2~ Three times, all the air in the autoclave was replaced with nitrogen.

[0036] 3) Turn on the cooling water in the jacket of the autoclave, control the temperature in the autoclave to belo...

Embodiment 3

[0042] 1) Dissolve 75g (0.49mol) of 3-methoxy-4-hydroxybenzaldehyde in 300g of anhydrous methanol in advance for later use.

[0043] 2) Pump the 3-methoxyl-4-hydroxybenzaldehyde solution ready for use in step 1) into a 1L autoclave, start stirring, add 9.4g of Raney nickel catalyst, and then add 220g of anhydrous methanol , close all the valves of the autoclave, first take away most of the air with vacuum, and then introduce nitrogen until the pressure in the autoclave reaches 3kg / c㎡, and there is no change in the pressure, confirm that the seal of the autoclave is intact, and then discharge the nitrogen, repeat the operation 2~ Three times, all the air in the autoclave was replaced with nitrogen.

[0044] 3) Turn on the cooling water in the jacket of the autoclave, control the temperature in the autoclave to below 35°C, add 225g (13.2mol) of liquid ammonia to the autoclave, and the rate of adding liquid ammonia is to control the temperature in the autoclave to below 50°C.

...

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 preparation method of 3-methoxy-4-hydroxybenzylamine hydrochloride. According to the method, 3-methoxy-4-hydroxybenzaldehyde reacts with liquid ammonia and hydrogen at the reaction temperature of 45-50 DEG C with a methanol solvent and a raney nickel catalyst, a product 3-methoxy-4-hydroxybenzylamine is obtained and dissolved in a methanol solvent, the mixture reacts with hydrogen chloride at the room temperature, and 3-methoxy-4-hydroxybenzylamine hydrochloride is obtained. Hydroxylamine hydrochloride in the traditional synthetic process of 3-methoxy-4-hydroxybenzylamine hydrochloride is replaced with the liquid ammonia, the product yield is increased, the adopted raw materials are easy to obtain, the methanol solvent can be recycled, and the raw material cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical reagent synthesis technology, and in particular relates to a preparation method of 3-methoxy-4-hydroxybenzylamine hydrochloride. Background technique [0002] 3-Methoxy-4-hydroxybenzylamine hydrochloride is a pharmaceutical intermediate, a key intermediate for the synthesis of natural capsaicinoids and their analogues, and can also be used as a food additive. [0003] The traditional 3-methoxyl-4-hydroxybenzylamine hydrochloride preparation process mainly contains the following two kinds: one is to synthesize by Leuckart (Leuckart) reaction, but this reaction needs to be carried out under high temperature conditions, and the reaction conversion rate is low The second is to use 3-methoxy-4-hydroxybenzaldehyde to react with hydroxylamine hydrochloride, then through catalytic hydrogenation reaction, and then refine, the synthesis process has low yield and high cost. Contents of the invention [0...

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): C07C217/64C07C213/00
Inventor 包泉兴成家钢方日青
Owner 黄石市利福达医药化工有限公司
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