Mandelic acid drug intermediate benzaldehyde synthesis method

A synthesis method and technology of benzaldehyde, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve the problems of high reaction energy consumption, complex synthesis process, high risk factor, etc., and achieve an increase in reaction yield , Improve the reaction yield and reduce the risk factor

Inactive Publication Date: 2018-07-03
CHENGDU QIESITE TECH CO LTD
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis method needs to react under pressurized conditions, and the reaction energy consumption is relatively high. The reaction process requires carbon monoxide and hydrogen chloride as reactants. The process is relatively complicated, so it is necessary to propose a new synthetic method

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
  • Mandelic acid drug intermediate benzaldehyde synthesis method
  • Mandelic acid drug intermediate benzaldehyde synthesis method
  • Mandelic acid drug intermediate benzaldehyde synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The synthetic method of mandelic acid medicine intermediate benzaldehyde comprises the steps:

[0019] A. Add 2mol of 1-aminomethyl-6-hydroxybenzene and 1.3L of potassium chloride solution with a mass fraction of 20% in the reaction vessel, control the stirring speed to 210rpm, increase the temperature to 60°C, keep reflux for 80min, and reduce When the temperature reaches 30°C, add 3 mol of a 40% glycerol diacetate solution;

[0020] B. Add 2 mol of lutetium oxide in 3 times within 30 minutes, continue to react for 60 minutes, add 10% potassium nitrate solution in mass fraction, let stand for stratification, take out oil layer, wash with 50% amyl formate solution with mass fraction, Wash with 60% chloroacetonitrile solution, recrystallize in 80% 2-chloroethanol solution, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain 186.55 g of finished benzaldehyde with a yield of 88%.

Embodiment 2

[0022] The synthetic method of mandelic acid medicine intermediate benzaldehyde comprises the steps:

[0023] A. Add 2mol of 1-aminomethyl-6-hydroxybenzene into the reaction vessel, 1.3L of 23% potassium chloride solution by mass fraction, control the stirring speed to 230rpm, raise the temperature to 63°C, keep reflux for 90min, and lower the temperature To 33°C, add 3.5 mol of 42% glycerol diacetate solution;

[0024] B. Add 2.5mol of lutetium oxide in 5 times within 40min, continue to react for 70min, add mass fraction and be 12% potassium nitrate solution, let stand for stratification, take out the oil layer, wash with 53% amyl formate solution with mass fraction, Wash with 63% chloroacetonitrile solution, recrystallize in 83% 2-chloroethanol solution, and dehydrate with anhydrous calcium sulfate dehydrating agent to obtain 195.04 g of finished benzaldehyde with a yield of 92%.

Embodiment 3

[0026] The synthetic method of mandelic acid medicine intermediate benzaldehyde comprises the steps:

[0027] A. Add 2mol of 1-aminomethyl-6-hydroxybenzene into the reaction vessel, 1.3L of 26% potassium chloride solution by mass fraction, control the stirring speed to 250rpm, raise the temperature to 68°C, keep reflux for 110min, lower the temperature To 37°C, add 4 mol mass fraction of 45% glycerol diacetate solution;

[0028] B. Add 3 mol of lutetium oxide in 7 times within 50 minutes, continue to react for 80 minutes, add 15% potassium nitrate solution in mass fraction, let stand for stratification, take out oil layer, wash with 57% amyl formate solution in mass fraction, Wash with 66% chloroacetonitrile solution, recrystallize in 87% 2-chloroethanol solution, and dehydrate with anhydrous potassium carbonate dehydrating agent to obtain 199.28 g of finished benzaldehyde with a yield of 94%.

[0029] For finished benzaldehyde 13 C NMR analysis, the analysis spectrum is as ...

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 discloses a mandelic acid drug intermediate benzaldehyde synthesis method, which comprises: adding 1-aminomethyl-6-hydroxybenzene and a potassium chloride solution in a reaction container, controlling the stirring speed, increasing the temperature, maintaining reflux, reducing the temperature, and adding a diacetin solution; adding lutetium oxide in batches, continuously carrying outthe reaction, adding a potassium nitrate solution, carrying out standing layering, taking out the oil layer, washing with an amyl formate solution, washing with a chloroacetonitrile solution, re-crystallizing in a 2-chloroethanol solution, and dehydrating with a dehydrating agent to obtain the finished product benzaldehyde.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, belonging to the field of organic synthesis, in particular to a synthesis method of benzaldehyde, a mandelic acid pharmaceutical intermediate. Background technique [0002] Benzaldehyde is an important raw material in medicine, dyestuff, perfume and resin industry, and can be used as solvent, plasticizer and low-temperature lubricant, etc. In the flavor industry, it is mainly used to prepare food flavors, and a small amount is used in daily chemical flavors and tobacco flavors. Although widely used as a commercial food flavoring and industrial solvent, benzyl alcohol's primary use is in the synthesis of a variety of other compounds ranging from pharmaceuticals to plastic additives. Benzyl alcohol is also an important intermediate product in the production of perfumes, fragrances and the synthesis of certain aniline dyes. The synthesis of mandelic acid uses benzaldehyde as...

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): C07C45/00C07C47/54
CPCC07C45/00C07C47/54
Inventor 彭飞
Owner CHENGDU QIESITE TECH CO LTD
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