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

Preparing method of 3-hydroxypropionic acid ester

A hydroxypropionate and quinoline-based technology, applied in the field of preparation of 3-hydroxypropionate, can solve problems such as difficult separation of catalysts, and achieve the effects of mild catalytic reaction conditions, resolution of separation difficulties, and high activity

Inactive Publication Date: 2017-02-22
CHINA PETROLEUM & CHEM CORP +1
View PDF7 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] What the present invention aims to solve is the problem that the homogeneous system catalyst in the prior art is difficult to separate, and provides a new preparation method of 3-hydroxypropionate, which has the advantage that the catalyst system is easily separated from the reaction system

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
  • Preparing method of 3-hydroxypropionic acid ester
  • Preparing method of 3-hydroxypropionic acid ester
  • Preparing method of 3-hydroxypropionic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Synthesis of ligand A

[0037]

[0038] Into a 100mL round-bottomed flask, add 5.0g of gel-type chloromethylated polystyrene resin (1% divinylbenzene cross-linked, chlorine content of 4.0mmol / g), 0.2mol of 2-hydroxypyridine, 0.2mol of Cesium carbonate and 200 mL of dioxane were reacted under reflux for 72 hours. The reaction was completed, suction filtration, washed the solid with 20 mL of dioxane for many times, then washed the solid with 20 mL of deionized water for many times, and finally washed the solid with 20 mL of ethanol and 20 mL of diethyl ether for many times, and vacuum-dried to obtain 5.87g of light yellow solid. It is ligand A (nitrogen content is 2.0 mmol / g).

[0039] 2. Synthesis of methyl 3-hydroxypropionate

[0040] 1.0 mmol of Co 2 (CO) 8 It was dissolved in 740 mmol of methanol, 1 g of ligand A was added, and the mixture was stirred at room temperature for 2 hours. The catalyst solution was transferred to a 100 mL reactor, the reactor was...

Embodiment 2

[0043] 1. Synthesis of ligand B

[0044]

[0045] In a 100mL round-bottomed flask, add 5.0g of gel-type chloromethylated polystyrene resin (1% divinylbenzene cross-linked, chlorine content of 4.0mmol / g), 0.2mol of 3-hydroxypyridine, 0.2mol of Cesium carbonate and 200 mL of dioxane were reacted under reflux for 72 hours. The reaction was completed, suction filtration, washed the solid with 20 mL of dioxane for many times, then washed the solid with 20 mL of deionized water for many times, and finally washed the solid with 20 mL of ethanol and 20 mL of diethyl ether for many times, and vacuum-dried to obtain 5.87g of light yellow solid. It is ligand B (nitrogen content is 2.2mmol / g).

[0046] 2. Synthesis of methyl 3-hydroxypropionate

[0047] 1.0 mmol of Co 2 (CO) 8 It was dissolved in 740 mmol of methanol, 0.91 g of ligand B was added, and the mixture was stirred at room temperature for 2 hours. The catalyst solution was transferred to a 100 mL reactor, the reactor was p...

Embodiment 3

[0050] 1. Synthesis of ligand C

[0051]

[0052] In a 100mL round-bottomed flask, add 5.0g of gel-type chloromethylated polystyrene resin (1% divinylbenzene cross-linked, chlorine content of 4.0mmol / g), 0.2mol of 4-hydroxypyridine, 0.2mol of Cesium carbonate and 200 mL of dioxane were reacted under reflux for 72 hours. The reaction was completed, suction filtration, washed the solid with 20 mL of dioxane for many times, then washed the solid with 20 mL of deionized water for many times, and finally washed the solid with 20 mL of ethanol and 20 mL of diethyl ether for many times, and vacuum-dried to obtain 5.87g of light yellow solid. It is ligand C (nitrogen content is 2.5mmol / g).

[0053] 2. Synthesis of methyl 3-hydroxypropionate

[0054] 1.0 mmol of Co 2 (CO) 8 It was dissolved in 740 mmol of methanol, 0.8 g of ligand C was added, and the mixture was stirred at room temperature for 2 hours. The catalyst solution was transferred to a 100 mL reactor, the reactor was ...

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 relates to a preparing method of 3-hydroxypropionic acid ester, and aims to solve the problem that a catalyst under a homogeneous system is difficult to separate in the prior art. The preparing method of the 3-hydroxypropionic acid ester comprises the steps of making ligand and cobalt carbonyl conduct coordination reaction in a solvent to obtain catalyst solution, wherein the solvent is alcohol or a solvent containing the alcohol, the ligand comprises a crosslinked polystyrene skeleton and -CH2XR perssad which is connected to benzene ring in the crosslinked polystyrene skeleton, wherein X is chosen from one of O atom, S atom and NH radical, R is chosen from one of 2-pyridyl, 3-pyridyl, 4-pyridyl, 5-quinolyl, 6-quinolyl, 7-quinolyl and 8-quinolyl; adding ethylene oxide and carbon monoxide into the catalyst solution to conduct reaction so as to obtain the 3-hydroxypropionic acid. According to the technical scheme, technical problems are favorably solved, and the preparing method can be applicable to the industrial production of 3-hydroxypropionic acid ester.

Description

technical field [0001] The present invention relates to a preparation method of 3-hydroxypropionate. Background technique [0002] 1,3-Propanediol is an important organic fine chemical that can be used as a raw material for the production of antifreeze, plasticizer, preservative and emulsifier, and is also widely used in food, cosmetics and pharmaceutical industries. The application is to synthesize polytrimethylene terephthalate (PTT) polyester fiber as a monomer. Compared with the commonly used polyethylene terephthalate (PET) fiber, PTT fiber has both light resistance, less water absorption and stability It has excellent properties such as good performance, good resilience, easy biodegradation and little environmental pollution. It has a wide range of application prospects and is the focus of current research and development. At present, there are three main processes for 1,3-propanediol: the ethylene oxide hydroformylation hydrogenation method developed by Shell Company...

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): C07C69/675C07C67/37B01J31/22
CPCC07C67/37B01J31/22B01J2531/845C07C69/675
Inventor 刘波吕建刚金照生李晓明孙兰萍
Owner CHINA PETROLEUM & CHEM CORP
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