Method for preparing adamantly alkyl vinyl ether
A kind of technology of adamantyl alkyl ethylene and its manufacturing method, which is applied in the direction of preparation of ether, addition of unsaturated compound to ether, organic chemistry, etc., can solve the problem of high conversion rate of adamantanol in one pass of acetylene conversion rate, and achieve high purity, The effect of stable reaction and high conversion rate
Inactive Publication Date: 2012-10-31
重庆市化工研究院有限公司
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[0005] The purpose of the present invention is to overcome the shortcomings of using highly toxic chemicals and polluting environmental substances in the above-mentioned manufacturing method, and provide a new green synthesis process of adamantyl alkyl vinyl ether, which has good reaction safety and reliability, acetylene conversion rate and adamantine High alkanol conversion per pass
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[0017] Example 1 100.0g (99.5%) of 1-adamantanemethanol, 50.0g of potassium tert-butylate, 5.0g of potassium hydroxide, and 500ml of alkane solvent were added to the autoclave, and acetylene (99.5%) gas was fed from the bottom to keep the pressure at React at 160°C for 4 hours at 1.0 MPa, lower the temperature, filter out the catalyst, distill the solvent, cool and crystallize, and recrystallize the crystals with anhydrous methanol twice or more to obtain 90.0 g of the product (light yellow crystals), the product purity is 99.58%, 1- The one-pass conversion rate of adamantane methanol is 77.8%.
[0018] Example 2 50.0g (99.6%) of 1-adamantane ethanol, 40.0g of potassium tert-butylate, 5.0g of potassium hydroxide, and 500ml of alkane solvent were added into the autoclave, and acetylene (99.5%) gas was fed from the bottom, and the pressure was kept at React at 160°C under 1.0MPa for 4 hours until the pressure of acetylene does not drop, lower the temperature, filter out the cata...
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The invention discloses a method for preparing adamantly alkyl vinyl ether. The method comprises the steps of: taking adamantanol and acetylene as raw materials, potassium alcoholate and potassium hydroxide as catalysts, and hydrocarbon as a solvent to react in a high-pressure autoclave, so as to obtain the adamantly alkyl vinyl ether, adding the adamantanol, the solvent and the catalysts once, leading acetylene gas from the bottom part after replacing nitrogen, reacting for 2-8 hours under the condition that the temperature is 100-180 DEG C and the pressure is 0.1-2.0MPa, cooling, filtering the catalysts, distilling out the solvent by filtrate, and distilling under reduced pressure to obtain the product or cooling and crystallizing, re-crystallizing the crystal more than twice by alcohol or ether solvent to obtain the product, wherein the purity of the product is more than 99.5%, and the conversion per pass of the adamantanol is 70-98%. The adamantly alkyl vinyl ether is mainly applied to the field of photoresist.
Description
technical field [0001] The present invention relates to a kind of production method of adamantyl alkyl vinyl ether. Background technique [0002] The integrated circuit industry is a country's fundamental and critical industry. As the leader of the integrated circuit industry, the development of lithography technology is even more important, because it directly determines the physical size of a single device. The emergence of each new generation of integrated circuits always takes the line width obtained by lithography as the main technical symbol. Photoresist is a key material required for the photolithography process. With the development of the integrated circuit industry, it has also experienced from G-line (436nm) lithography, I-line (365nm) lithography, deep ultraviolet 248nm lithography, to the present The development history of 193nm lithography. In the high-end field of photoresist, the technology has been monopolized by American and Japanese manufacturers. Sever...
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IPC IPC(8): C07C43/178C07C43/162C07C41/08
Inventor 赵丽颖颜邦民吴渝蒋惠李昌杰李刚
Owner 重庆市化工研究院有限公司