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Preparation method for 2-ethyl-2-adamantanol methacrylate

A technology of adamantanol methacrylate and methacryloyl chloride, applied in the preparation of carboxylic acid halides, organic chemistry, etc., can solve the problems of complicated separation process, obtaining pure products, difficult cost control, etc., and achieve simple separation process , high product purity and less by-products

Active Publication Date: 2015-05-20
XUZHOU B&C CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Alkyl adamantyl esters obtained by known methods in the prior art often produce a large amount of impurities due to too many side reactions, resulting in complicated separation processes, and cannot obtain pure products by crystallization, etc., resulting in low yields and difficult costs. control, which also directly makes it difficult to be applied to industrial production

Method used

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  • Preparation method for 2-ethyl-2-adamantanol methacrylate
  • Preparation method for 2-ethyl-2-adamantanol methacrylate
  • Preparation method for 2-ethyl-2-adamantanol methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064]Step 1. Dissolve 500g of adamantanone in 1550ml of anhydrous tetrahydrofuran, add 500g of bromoethane under stirring, and stir until completely dissolved under nitrogen protection.

[0065] Step 2. Add 50g of lithium metal and 450ml of anhydrous tetrahydrofuran (water content less than 200ppm) into a 5000ml reaction bottle with mechanical stirring, and drop the temperature to -5°C to 0°C while stirring, and start adding the above mixed solution for about 7 hours. After finishing, control the temperature at 10°C to 20°C.

[0066] Step 3. After dripping, keep warm for 1 hour, then remove the cooling equipment and naturally rise to room temperature (20°C-25°C) and stir for about 14 hours. After sampling, add water to quench the reaction, TLC, and send the sample to GC after passing the test (central control 1).

[0067] Step 4: After cooling down to -10°C to -8°C, add 5g of phenothiazine and start dropping 418g of methacryloyl chloride to control the rate of addition and co...

Embodiment 2

[0074] Step 1. Dissolve 150g of adamantanone in 370ml of anhydrous benzene, add 120g of ethyl bromide under stirring, and stir until completely dissolved under nitrogen protection.

[0075] Step 2: Add 38.4g of magnesium metal and 190ml of anhydrous benzene into a 1000ml reaction bottle with mechanical stirring, and drop the temperature to -5°C to 0°C while stirring, start adding the above mixed solution dropwise for about 5 hours, and control the temperature Between 10°C and 20°C.

[0076] Step 3. After dripping, keep warm for 1 hour, then remove the cooling equipment and naturally rise to room temperature (20°C-25°C) and stir for about 12 hours. After sampling, add water to quench the reaction, TLC, and send the sample to GC after passing the test (central control 1).

[0077] Step 4: After cooling down to -10°C to -8°C, add 4.5g of 1,4-naphthoquinone and start adding 166g of methacryloyl chloride dropwise to control the rate of addition and control the temperature at -10°C ...

Embodiment 3

[0084] Step 1. Dissolve 150g of adamantanone in 300ml of anhydrous tetrahydrofuran, add 196g of bromoethane under stirring, and stir until completely dissolved under nitrogen protection.

[0085] Step 2. Add 17.5g of lithium metal and 60ml of anhydrous tetrahydrofuran into a 1000ml reaction bottle with mechanical stirring, and drop the temperature to -5°C to 0°C while stirring, and start adding the above mixed solution dropwise for about 10 hours. Control the temperature Between 10°C and 20°C.

[0086] Step 3. After dripping, keep warm for 1.5 hours, then remove the cooling equipment and naturally rise to room temperature (20°C-25°C) and stir for about 10 hours. After sampling, add water to quench the reaction, TLC, and send the sample to GC after passing the test (central control 1).

[0087] Step 4: After cooling down to -10°C to -8°C, add 2.5g of phenothiazine and start to drop 104g of methacryloyl chloride to control the rate of addition and control the temperature at -10°...

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Abstract

The invention provides a preparation method for 2-ethyl-2-adamantanol methacrylate. The method is characterized by including the steps of: adding bromoethane into adamantanone of a solvent dropwise to form a No.1 preparatory solution; placing a metal into the solvent to form a No.2 preparatory solution; adding the No.1 preparatory solution into the No.2 preparatory solution slowly in a dropwise manner; raising the temperature to room temperature naturally and carrying out reaction for 10-20h; under a system temperature below 0DEG C, adding a polymerization inhibitor, and adding methacryloyl chloride dropwise; raising the temperature to room temperature naturally and carrying out reaction for 10-20h; adding water to carry out quenching reaction; and performing aftertreatment to obtain 2-ethyl-2-adamantanol methacrylate. According to the synthesis method provided by the invention, by selecting the reaction conditions of each step, like reaction temperature, reactant ratio, reaction time, reaction feedstock and the like, the problems of difficult purification, too high cost, low reaction yield, low product purity, inapplicability to large-scale industrial production and the like in existing technical disclosure can be overcome.

Description

technical field [0001] The invention relates to the field of organic synthesis, and particularly provides a preparation method of 2-ethyl-2-adamantanol methacrylate. Background technique [0002] Adamantane is a regular, symmetrical and highly stable cage-like hydrocarbon. Because it has a structure in which four cyclohexane rings are condensed into a cage-like structure, it is a highly symmetrical and stable compound. It is known that its derivatives are involved in the fields of medicine, aerospace, functional materials, petroleum processing and so on. [0003] It is worth mentioning that adamantane has properties such as optical properties and heat resistance, so its derivatives are often used in optical disc substrates, optical fibers or lens lamps. It can be used as a photoresist for semiconductors, a sealing agent for optical semiconductors, optical and electronic components (light pipes, optical communication lenses, optical films, etc.) and their adhesives. [0004...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/14
CPCC07C67/14C07C2603/74C07C69/54
Inventor 傅志伟
Owner XUZHOU B&C CHEM CO LTD
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