Method for selectively synthesizing 3-nitrosalicylic acid in continuous flow region

A technology of nitrosalicylic acid and salicylic acid, which is applied in chemical instruments and methods, preparation of nitro compounds, preparation of organic compounds, etc., can solve the problem of long post-treatment time of 3-nitrosalicylic acid and failure to meet the aging requirements Requirements, easy to generate other by-products and other issues, to achieve the effect of less side reactions, fast reaction speed, improved yield and purity

Active Publication Date: 2021-03-23
ASTATECH CHENGDU BIOPHARM CORP
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The nitration selectivity of the methyl cylate nitration method is low, and other by-products are easily generated; and the method obtains 3-nitrosalicylic acid through a two-step reaction and takes a long time for the reaction and aftertreatment, and the operation is loaded down with trivial details and the yield is low, which cannot satisfy The timeliness of the market

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 selectively synthesizing 3-nitrosalicylic acid in continuous flow region
  • Method for selectively synthesizing 3-nitrosalicylic acid in continuous flow region
  • Method for selectively synthesizing 3-nitrosalicylic acid in continuous flow region

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1, the method for continuous flow regioselective synthesis of 3-nitrosalicylic acid of the present invention

[0048] refer to figure 1 As shown in the process flow diagram, a microchannel reactor is utilized to synthesize 3-nitrosalicylic acid. Specific steps are as follows:

[0049] 1) Measure 900mL 99% acetic acid, 2.5g Prussian blue, and 100g salicylic acid into 2L beaker A respectively to obtain material 1; weigh 104.4g of concentrated nitric acid with a mass fraction of 65% and pour into 200mL beaker B to obtain Material 2.

[0050] 2) Connect beaker A and beaker B to metering pump P1 and metering pump P2 respectively; start metering pump P1 first, feed material 1 to the preheating module, and preheat at 50°C for 1 minute.

[0051] 3) Then start the metering pump P2, feed the material 2 and the preheated material 1 to the mixing module at the same time, and obtain the material 3 after mixing evenly in the mixing module; the temperature of the mixing ...

Embodiment 2

[0054] Embodiment 2, the method for continuous flow regioselective synthesis of 3-nitrosalicylic acid of the present invention

[0055] refer to figure 1 As shown in the process flow diagram, a microchannel reactor is utilized to synthesize 3-nitrosalicylic acid. Specific steps are as follows:

[0056] 1) Measure 900mL 99% acetic acid, 2.5g Prussian blue, and 100g salicylic acid into 2L beaker A respectively to obtain material 1; weigh 104.4g of concentrated nitric acid with a mass fraction of 65% and pour into 200mL beaker B to obtain Material 2.

[0057] 2) Connect beaker A and beaker B to metering pump P1 and metering pump P2 respectively; start metering pump P1 first, feed material 1 to the preheating module, and preheat at 35°C for 1 minute.

[0058] 3) Then start the metering pump P2, feed the material 2 and the preheated material 1 to the mixing module at the same time, and obtain the material 3 after mixing evenly in the mixing module; the temperature of the mixing ...

Embodiment 3

[0061] Embodiment 3, the method for continuous flow regioselective synthesis of 3-nitrosalicylic acid of the present invention

[0062] refer to figure 1 As shown in the process flow diagram, a microchannel reactor is utilized to synthesize 3-nitrosalicylic acid. Specific steps are as follows:

[0063] 1) Measure 900mL of 99% acetic acid, 2.5g of zirconia-silicotungstic acid, and 100g of salicylic acid into 2L beaker A to obtain material 1; weigh 104.4g of concentrated nitric acid with a mass fraction of 65% and pour into a 200mL beaker In B, material 2 was obtained.

[0064] 2) Connect beaker A and beaker B to metering pump P1 and metering pump P2 respectively; start metering pump P1 first, feed material 1 to the preheating module, and preheat at 50°C for 1 minute.

[0065] 3) Then start the metering pump P2, feed the material 2 and the preheated material 1 to the mixing module at the same time, and obtain the material 3 after mixing evenly in the mixing module; the temper...

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

PropertyMeasurementUnit
quality scoreaaaaaaaaaa
quality scoreaaaaaaaaaa
Login to view more

Abstract

The invention provides a method for selectively synthesizing 3-nitrosalicylic acid in a continuous flow region. According to the method, salicylic acid and nitric acid are used as raw materials and react in a micro-channel reactor in the presence of a catalyst and a reaction solvent to synthesize the 3-nitrosalicylic acid. The method for synthesizing the 3-nitrosalicylic acid is high in reaction speed, few in side reaction, high in heat and mass transfer efficiency, high in reaction selectivity, convenient in post-treatment, high in product purity and high in yield, and has a wide applicationprospect in industrial synthesis of the 3-nitrosalicylic acid.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a continuous-flow region-selective synthesis method for 3-nitrosalicylic acid. Background technique [0002] 3-Nitrosalicylic acid is a raw material for organic synthesis and an important intermediate for the preparation of various therapeutic drugs. For example, 3-nitrosalicylic acid is an important intermediate for the preparation of novel 3,4-diamino-3-cyclobutene-1,2-dione compounds, the novel 3,4-diamino-3-cyclobutene En-1,2-dione compounds are drugs for the treatment of chemokine-mediated diseases; 3-nitrosalicylic acid is a synthetic 4,5-diamino-1,2,3,4-tetrahydro-3,6 - an important intermediate of pyridazinone, 4,5-diamino-1,2,3,4-tetrahydro-3,6-pyridazinone is a drug for the treatment of inflammatory diseases and cancer; 3-nitrosalicylic acid The acid is also an important intermediate for the preparation of novel antimycin A3 analogs. [0003] At present,...

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 Applications(China)
IPC IPC(8): C07C201/08C07C205/60C07C201/16
CPCC07C201/08C07C201/16C07C205/60Y02P20/584
Inventor 赵振宇王银姜青龙王智郭鹏
Owner ASTATECH CHENGDU BIOPHARM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap