CN109836424B - Method for preparing caffeine by methylation of environment-friendly theophylline sodium salt - Google Patents
Method for preparing caffeine by methylation of environment-friendly theophylline sodium salt Download PDFInfo
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- CN109836424B CN109836424B CN201910184371.2A CN201910184371A CN109836424B CN 109836424 B CN109836424 B CN 109836424B CN 201910184371 A CN201910184371 A CN 201910184371A CN 109836424 B CN109836424 B CN 109836424B
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Abstract
本发明为一种环保型茶碱钠盐甲基化制备咖啡因的方法。该方法包括以下步骤:向反应釜加入茶碱钠盐,DMC,甲醇,在100‑180℃、搅拌下,反应1‑5小时;待冷却后通过旋转蒸发进行分离,得到的固体即粗品咖啡因。本发明大大提高茶碱钠盐与DMC甲基化反应的反应效率,并通过简单的提纯步骤,将制得的粗品咖啡因进行提纯;咖啡因收率最高可达97.3%。The present invention is an environment-friendly method for preparing caffeine by methylation of sodium salt of theophylline. The method comprises the following steps: adding theophylline sodium salt, DMC, and methanol to the reaction kettle, and reacting at 100-180° C. under stirring for 1-5 hours; after cooling, it is separated by rotary evaporation, and the obtained solid is crude caffeine . The invention greatly improves the reaction efficiency of the methylation reaction between theophylline sodium salt and DMC, and through simple purification steps, the obtained crude caffeine is purified; the maximum caffeine yield can reach 97.3%.
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CN109836424B true CN109836424B (en) | 2022-04-01 |
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CN114315833A (en) * | 2020-09-27 | 2022-04-12 | 天津药业研究院股份有限公司 | Method for synthesizing caffeine |
CN112724143B (en) * | 2021-02-07 | 2022-04-15 | 河北工业大学 | A kind of method for preparing theobromine by methylation of 3-methylxanthine |
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CN104892611B (en) * | 2015-05-19 | 2017-03-22 | 青岛科技大学 | Synthetic method of caffeine |
CN105294691B (en) * | 2015-11-23 | 2017-03-08 | 青岛科技大学 | A kind of preparation technology of environment-friendly semi-synthetic caffeine |
CN106046004B (en) * | 2016-06-06 | 2018-05-15 | 上海佰特因医药科技有限公司 | A kind of total synthesis method of 1,3,7,9- tetramethyluric acids |
CN106496227A (en) * | 2016-08-31 | 2017-03-15 | 安徽省润生医药股份有限公司 | A kind of preparation method and its usage of istradefylline |
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Inventor after: Xue Wei Inventor after: Yang Hansen Inventor after: Feng Zhijun Inventor after: Xie Lisha Inventor after: Zhang Min Inventor after: Li Fang Inventor after: Zhang Dongsheng Inventor after: Wang Yanji Inventor before: Xue Wei Inventor before: Yang Hansen Inventor before: Feng Zhijun Inventor before: Xie Lisha Inventor before: Li Fang Inventor before: Zhang Dongsheng Inventor before: Wang Yanji |
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Effective date of registration: 20250613 Address after: 300000 Tianjin City Binhai New Area Airport Economic Zone Huabei Road Business Park West District Building No.1 8th Floor Patentee after: TIANJIN HAOYONG CHEMICAL ENGINEERING Co.,Ltd. Country or region after: China Address before: 300130 Tianjin city Hongqiao District dingzigu glorious road No. 8 Eastern Hospital of Hebei University of Technology 330# Patentee before: Hebei University of Technology Country or region before: China |