Synthesis method of single-ended unsaturated polyethylene glycol compound

A polyethylene glycol and synthesis method technology, applied in the field of organic synthesis, can solve problems such as danger, high requirements for storage conditions, and high requirements for experimental equipment, and achieve the effects of reducing equipment requirements, reducing production costs, and improving product purity

Pending Publication Date: 2021-11-23
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These strong bases and elemental metals are expensive and dangerous, and require high storage conditions; in addition, during the reaction process, the temperature will continue to rise after the reaction is initiated and the temperature will rise relatively rapidly, and it will increase with the increase of the amount, so that the overall reaction is at Under the environment of high temperature and high pressure, the requirements for experimental equipment are relatively high, and the risk is very high, so it is not suitable for promotion to industrial production

Method used

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  • Synthesis method of single-ended unsaturated polyethylene glycol compound
  • Synthesis method of single-ended unsaturated polyethylene glycol compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: take potassium hydride, potassium hydroxide as initiator

[0030] Add 50mL of anhydrous tetrahydrofuran to the reactor, add 1.78g of potassium hydride and 1g of potassium hydroxide, close the reactor, fill the reactor with nitrogen to pressurize, then vacuumize and then fill with nitrogen; open the vent valve, and then open the feed valve, add 1.17g of 2-methallyl alcohol, close the feed valve, then close the vent valve, turn on the stirring, set the temperature at 40°C, react for four hours, turn off the stirring, heat, and cool the reactor with liquid nitrogen To minus 20°C, vacuumize and then fill with nitrogen, repeat this three times; open the vent valve, then open the feed valve, carefully add ethylene oxide (100mL) and quickly close the feed valve and vent valve, put Set the temperature at 45°C and react for three days. After the reaction time is up, evaporate the solvent to dryness; add 100 mL of 0.5 mol / L hydrochloric acid solution and stir for 30...

Embodiment 2

[0034] With sodium hydride and potassium hydroxide as initiators, the chemical equation is as follows:

[0035]

[0036] Add 50mL of anhydrous tetrahydrofuran to the reactor, add 2.61g of sodium hydride and 1g of potassium hydroxide, close the reactor, pressurize the reactor with nitrogen, then vacuumize and then fill with nitrogen; open the vent valve, and then open the feed valve, add 1.71g of 2-methallyl alcohol, close the feed valve, then close the release valve, turn on the stirring, and set the temperature to 40°C. React for four hours, turn off stirring and heating, cool the reactor to minus 20°C with liquid nitrogen, vacuumize and then fill with nitrogen, repeat this three times; open the vent valve, then open the feed valve, and carefully add ethylene oxide After alkane (100mL), quickly close the feed valve and vent valve, set the temperature to 45°C and react for three days, after the reaction time is up, evaporate the solvent to dryness; add 0.5mol / L hydrochloric...

Embodiment 3

[0039] Embodiment 3: take sodium hydride, potassium hydroxide as initiator

[0040]50 mL of anhydrous tetrahydrofuran was added to the reactor, and 1.06 g of sodium hydride and 1 g of potassium hydroxide were added. Close the reactor, pressurize the reactor with nitrogen and then evacuate and then fill with nitrogen; open the vent valve, then open the feed valve, add 2.91g of 2-methallyl alcohol, close the feed valve, and then close the discharge valve. Air valve, open the stirring, set the temperature at 40°C, react for four hours, turn off the stirring, heat, cool the reactor to minus 20°C with liquid nitrogen, and then fill it with nitrogen after vacuuming, repeat this three times; open the vent valve , and then open the feed valve, carefully add ethylene oxide (100mL) and quickly close the feed valve and vent valve, set the temperature to 45°C and react for three days, after the reaction time is reached, evaporate the solvent to dryness; add 100 mL of 0.5 mol / L hydrochlor...

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Abstract

The invention belongs to the technical field of organic synthesis, and discloses a synthesis method of a single-ended unsaturated polyethylene glycol compound. The method takes ethylene oxide and 2-methylallyl alcohol as reactants and takes mixed alkali as an initiator, and the single-ended unsaturated polyethylene glycol compound is prepared at normal temperature and normal pressure by controlling the adding sequence of materials. According to the preparation method, the specific mixed alkali which is low in price and relatively safe is adopted as the initiator to replace single strong alkali or alkali metal simple substance which is high in price and relatively dangerous, so that the preparation cost of the polyglycol ether with the methyl allyl at the single end position is greatly reduced, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and more specifically relates to a method for synthesizing single-end unsaturated polyethylene glycol compounds. Background technique [0002] Single-ended methallyl polyglycol ether is an important fine chemical intermediate and an important polymerization monomer of polycarboxylate water reducer. [0003] Polyethylene glycol is a highly hydrophilic polyether, easily soluble in organic solvents and water, has excellent physical, chemical and biological properties, and is non-toxic, non-antigenic and immunogenic, and is an additive that has been approved by the FDA to enter the human body , Polyethylene glycol has good biocompatibility, is non-toxic to the human body, and exhibits low protein and low platelet adsorption and low cell adhesion in the body. These characteristics make it widely used in the field of biomedicine, so it is used Modification of small molecule drugs is a hot ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2648
Inventor 娄大伟张跃伟祝波张浩
Owner JILIN INST OF CHEM TECH
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