Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of vitamin E polyethylene glycol monomethyl ether succinate

A technology of polyethylene glycol monomethyl ether and succinate, which is applied in the field of preparation of vitamin E polyethylene glycol monomethyl ether succinate, can solve the problems of low purity, improve purity and avoid the discharge of toxic solutions Effect

Active Publication Date: 2019-09-20
ZHEJIANG QIMING BIOCHEM TECH
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are many reports about the synthesis of vitamin E polyethylene glycol succinate in the current literature, but the synthetic method of vitamin E polyethylene glycol monomethyl ether succinate has only been reported in U.S. Patent No. 8,785,665. Volatile and toxic toluene is used as a reaction solvent, and a large amount of alumina is used as an adsorbent to absorb impurities, resulting in a large amount of solid waste
And the purity of vitamin E polyethylene glycol monomethyl ether succinate synthesized by the method is only 90%~97%.

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: A kind of preparation method of vitamin E polyethylene glycol monomethyl ether succinate, 310g polyethylene glycol monomethyl ether, 200g vitamin E succinate, 10g p-toluenesulfonic acid are added in 1000ml four-neck flask . Then start stirring, and after the stirring finishes, the four-necked flask is vacuumized so that the vacuum degree in the four-necked flask reaches -0.09Mpa. Then start to raise the temperature, and control the temperature at 110°C to 120°C for 7 hours to carry out the esterification reaction. After the reaction, the temperature of the reaction solution was lowered to 60-70°C, then 200 g of an aqueous sodium chloride solution with a mass of 20% sodium chloride was added, and then 200 g of a saturated sodium bicarbonate solution was added dropwise, and stirred for 30 minutes to separate the reaction solution. After pumping out the lower aqueous solution of the reaction solution, add 10g of medicinal charcoal and 50g of aluminum oxide t...

Embodiment 2

[0023] Embodiment 2: A kind of preparation method of vitamin E polyethylene glycol monomethyl ether succinate, 310g polyethylene glycol monomethyl ether, 200g vitamin E succinate, 20g p-toluenesulfonic acid are added in 1000ml four-neck flask . Then start stirring, and after the stirring finishes, the four-necked flask is vacuumized so that the vacuum degree in the four-necked flask reaches -0.09Mpa. Then start to raise the temperature, and control the temperature at 110°C to 120°C for 7 hours to carry out the esterification reaction. After the reaction, the temperature of the reaction solution was lowered to 60-70°C, then 200 g of an aqueous sodium chloride solution with a mass of 20% sodium chloride was added, and then 200 g of a saturated sodium bicarbonate solution was added dropwise, and stirred for 30 minutes to separate the reaction solution. After pumping away the aqueous solution of the lower layer of the reaction solution, add 10g of medicinal charcoal and 50g of ca...

Embodiment 3

[0024] Embodiment 3: A kind of preparation method of vitamin E polyethylene glycol monomethyl ether succinate, 330g polyethylene glycol monomethyl ether, 200g vitamin E succinate, 10g p-toluenesulfonic acid are added in 1000ml four-neck flask . Then start stirring, and after the stirring finishes, the four-necked flask is vacuumized so that the vacuum degree in the four-necked flask reaches -0.09Mpa. Then start to heat up, and control the temperature at 115°C to 125°C for 7 hours to carry out the esterification reaction. After the reaction, the temperature of the reaction solution was lowered to 60-70°C, then 200 g of an aqueous sodium chloride solution with a mass of 20% sodium chloride was added, and then 200 g of a saturated sodium bicarbonate solution was added dropwise, and stirred for 30 minutes to separate the reaction solution. After pumping away the aqueous solution of the lower layer of the reaction solution, add 10g of medicinal charcoal and 50g of hydrotalcite to ...

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
purityaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for preparing vitamin E methoxy polyethylene glycol succinate and relates to synthesis of compounds. The method comprises the following several steps: (A) subjecting vitamin E succinate and methoxy polyethylene glycol to an esterification reaction under the catalysis of an acidic catalyst, so as to form a reaction solution; (B) adding one or more inorganic salt solutions in the reaction solution, carrying out stirring, and then, subjecting the reaction solution to standing layering; (C) forming an upper-layer feed solution and a lower-layer aqueous solution after the standing layering of the reaction solution, pumping off the lower-layer aqueous solution, and adding an adsorbent in the upper-layer feed solution; (D) stirring the upper-layer feed solution, and then, carrying out filtration, thereby obtaining a filtrate, i.e., the vitamin E methoxy polyethylene glycol succinate. Compared with the prior art, the method has the advantages that no toluene or other reaction solvents is required to be added during preparation, so that the emission of a large volume of toxic solutions is avoided; and meanwhile, compared with the prior art, the method has the advantage that the purity of the prepared vitamin E methoxy polyethylene glycol succinate is further improved.

Description

technical field [0001] The invention relates to the synthesis of a compound, in particular to a preparation method of vitamin E polyethylene glycol monomethyl ether succinate. Background technique [0002] As a non-toxic non-ionic surfactant, vitamin E polyethylene glycol monomethyl ether succinate can form nano micelles in aqueous solution at room temperature to carry out organic chemical reactions, completely replacing the traditional process Use of large amounts of organic solvents. These nanomicelles are like nanoreactors that meet all the requirements of typical solvents used in chemical synthesis. The development of new catalytic systems that function in water in the presence of such surfactants will change the future of organic chemistry. At present, the reactions that these "tailor-made" surfactants can promote include: SNAr reaction, Peptide coupling, Suzuki-Miyaura coupling, nitro reduction, aryl amination reaction, Sonogashira coupling, carbon-hydrogen bond activ...

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 Patents(China)
IPC IPC(8): C08G65/332
Inventor 姜旭琦鲁承勇张晓华
Owner ZHEJIANG QIMING BIOCHEM TECH