2,2,6,6-四甲基-3,5-庚二酮的制备与纯化方式研究
Research on the Preparation and Purification Methods of 2,2,6,6-tetramethyl-3,5-heptanedione
吴峰1
作者信息
- 1. 博瑞生物医药泰兴市有限公司,江苏 泰兴 225400
- 折叠
摘要
以特戊酸甲酯和频呐酮作为主原料在缩合剂作用下制备2,2,6,6-四甲基-3,5-庚二酮(TMHD).实验筛选对比确定缩合剂,特戊酸甲酯和频呐酮的配比,后处理纯化方式,确定了适合工业化放大的工艺为叔丁醇钠作为缩合剂,配比在1.2～1.4 之间,采用溶析结晶方式就能得到纯度 99%以上的TMHD,比市售产品的纯度要高.且采用此方式回收率高,且不受精馏设备产能限制.
Abstract
2,2,6,6-tetramethyl-3,5-heptanedione(TMHD)was prepared using methyl valerate and pinalone as the main raw materials under the action of a condensing agent.Experimental screening and comparison were conducted to determine the ratio of condensing agent,methyl valproate,and pinalone,as well as the purification method for post-treatment.The suitable process for industrial scaling up was determined to be sodium tert butoxide as the condensing agent,with a ratio between 1.2 and 1.4.TMHD with a purity of over 99%can be obtained by dissolution crystallization,which is higher than the purity of commercially available products.And this method has a high recovery rate and is not limited by the production capacity of distillation equipment.
关键词
2,2,6,6-四甲基-3,5-庚二酮/工艺放大/缩合Key words
2,2,6,6-tetramethyl-3,5-heptanedione/process amplification/condensation引用本文复制引用
出版年
2024
NETL
NSTL
万方数据