Method for synthesizing MPC using one-pot method

A technology of mixing solution and acetonitrile, applied in the direction of phosphorus organic compounds, etc., can solve problems such as difficulty and difficulty in obtaining pure MPC, and achieve the effects of simple operation, saving input of raw materials and auxiliary materials, and saving equipment.

Inactive Publication Date: 2013-07-10
SUZHOU COSMETIC MATERIALS
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Problems solved by technology

At present, this method still has difficulties in product separation and purificat...

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  • Method for synthesizing MPC using one-pot method
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  • Method for synthesizing MPC using one-pot method

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Embodiment Construction

[0019] The present invention will be described in detail below in conjunction with embodiments.

[0020] The method for one-pot synthetic MPC, comprises the following steps:

[0021] Step 1) Dissolve 168g of phosphorus oxychloride (1.1eq) in 2500ml of acetonitrile, mix 62g of ethylene glycol (1.0eq) with 110g of triethylamine (1.1eq), and slowly add it dropwise to the above-mentioned acetonitrile at -10°C , then keep stirring at this temperature for 30 minutes, and stir at room temperature for one hour, then cool the reaction solution to -10°C;

[0022] Step 2) Slowly add a mixed solution of 117g HEMA (0.9eq) and 110g triethylamine (1.1eq) dropwise at -10°C, then stir at this temperature for three hours, cool to -20°C, and dissolve triethylamine under nitrogen protection. Filter out the amine hydrochloride, feed 180g trimethylamine (3.0eq) into the mother liquor, close the reactor, raise the temperature to 60°C and keep stirring at this temperature for 26 hours, spin dry the ...

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Abstract

The present invention discloses a method for synthesizing MPC using a one-pot method, comprising the following steps: step 1. dissolving phosphorus oxychloride in acetonitrile, slowly adding a mixture of ethylene glycol and triethylamine dropwise to the acetonitrile at -10 DEG C, stirring for 30 minutes at -10 DEG C, then stirring for one hour at room temperature, cooling the reaction solution to -10 DEG C; and step 2. slowly adding a mixed solution of hydroxyethyl methacrylate (HEMA) and triethylamine dropwise at -10 DEG C, stirring for three hours at -10 DEG C, cooling to -20 DEG C, removing triethylamine hydrochloride by filtration under a nitrogen atmosphere, feeding trimethylamine to a mother liquor, sealing a reactor, heating to 60 DEG C, keeping at the temperature and stirring for 26 hours continuously, evaporating solvents at 20 DEG C after cooling, adding acetone to give a solid powder, washing with acetonitrile, and filtering in presence of nitrogen. The method for synthesizing MPC using the one-pot method of the present invention is simple in operation, and helps to save a lot of inputs of devices and raw materials, reduce costs and provide a good direction for industrial production of MPC monomers.

Description

technical field [0001] The invention relates to a method for synthesizing MPC, in particular to a method for synthesizing MPC in one pot. Background technique [0002] Biocompatibility refers to the adaptability between materials implanted in animals and the body, including tissue compatibility and blood compatibility. Biomedical materials and various artificial organs and auxiliary devices implanted in the body must be non-toxic, non-sensitizing, non-irritating, non-genotoxic and non-carcinogenic, and must not cause harm to biological tissues, blood, immune systems, etc. Adverse reactions. Improving the biocompatibility of materials is an ultimate and general goal. There are various methods and means to improve biocompatibility through surface modification, which can be divided into two categories: methods of biological "activation" of surfaces and methods of "passivation" of surfaces. The approach to "activating" surfaces is to provide sites for recognition and specific...

Claims

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Application Information

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IPC IPC(8): C07F9/09
Inventor 凌静刘金永
Owner SUZHOU COSMETIC MATERIALS
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