Green Synthesis Applicable for Industrial-Scale Preparation of Efaproxiral Sodium
Green Synthesis Applicable for Industrial-Scale Preparation of Efaproxiral Sodium
复制标题
绿色合成适用于工业规模制备依普罗昔钠
DOI：
--
复制
发表时间：
2008
期刊：
影响因子：
--
通讯作者：
Yuefei Hu
中科院分区：
文献类型：
--
作者：
Hong;Jiajia Cao;Yuefei Hu
本文提出了一种新的合成方法，包括缩合和O-烷基化两步反应。在缩合步骤中，采用方便的方法来消除溶剂的使用，即，4-在150-180 °C下加热羟基苯乙酸和3，5-二甲基苯胺3-5小时，反应成功进行。苯胺在对羟基苯乙酸中的收率为90- 93%。在O-烷基化反应中，避免了以往的迂回工艺，直接得到了高质量的钠盐，收率达90%。最终产物依非替韦拉钠在水中结晶，得到一种新的晶体，其X射线粉末衍射图只有一个在2θ方向的3.7° ± 0.2°峰。最终产品质量高，经高效液相色谱检测含量为99.51%。本研究提供了一种环境友好、产率高、成本低、反应路线短的新工艺。
In this article we proposed a novel procedure for the synthesis of efaproxiral sodium, including two reaction steps, condensation, and O-alkylation. In the condensation step, a convenient method was adopted to eliminate the use of solvents, i.e., 4-hydroxyphenylacetic acid and 3,5-dimethylaniline were heated at 150-180 °C for 3-5 h, and the reaction was successfully carried out. The yield of anilide in 4-hydroxyphenylacetic acid was 90-93%. In the O-alkylation step, the old circuitous process was avoided, and high-quality sodium salt was directly obtained with a yield of 90%. The final product of efaproxiral sodium was crystallized in water, yielding a new crystalline form containing a unique X-ray powder diffraction pattern with only one peak of 3.7° ± 0.2° in 2θ. The quality of the final product is high with a content of 99.51% according to high-performance liquid chromatographic detection. The present study provided a new environmentally friendly procedure for the preparation of efaproxiral sodium with high yield, low cost, and a short reaction pathway.