贝诺酯合成工艺优化
Optimization of Benorilate Synthesis Process
赵莉娜 1刘方蕊 1李曼 1王智贤 1曹江营1
作者信息
- 1. 山东中医药大学药学院,山东济南 250355
- 折叠
摘要
以乙酰水杨酸为原料,氯化亚砜为氯代试剂,吡啶为催化剂,制得乙酰水杨酰氯.四氢呋喃为溶解乙酰水杨酰氯溶剂,TBAB为相转移催化剂,在5％氢氧化钠碱性条件下,对乙酰氨基酚与乙酰水杨酰氯缩合60 min,得到贝诺酯.对乙酰氨基酚和乙酰水杨酸的物质的量之比为1∶1.2.此工艺路线温和,后处理和纯化简单.总收率为69％.所得产物经过1H-NMR和13C-NMR确证结构.
Abstract
Using pyridine as the catalyst and sulfoxide chloride as the chlorinated reagent,acetylsalicylic acid underwent substitution reaction to give acetylsalicyloyl chloride.Then,using tetrahydrofuran as the solvent to dissolve the acetylsalicyloyl chloride and TBAB as the phase transfer catalyst,acetaminophen was condensed with acetylsalicyloyl chloride for 60 minutes to give benorilate under the alkaline condition of 5％sodium hydroxide.The mole ratio of acetaminophen to acetylsalicylic acid is 1∶1.2.The synthesis process is mild,with simple post-treatment and purification.The total yield is 69％.The target product was structurally confirmed by 1H-NMR and 13C-NMR.
关键词
贝诺酯/合成/优化/相转移催化剂Key words
benorilate/synthesis/optimization/phase transfer catalyst引用本文复制引用
基金项目
山东省医药卫生科技发展计划项目(202013051070)
山东中医药大学大学生创新训练计划项目(2023055)
出版年
2024
NETL
NSTL
万方数据