摘要
以三聚氯氰和叔辛胺为主要原料合成了光稳定剂944中间体4,6-二氯-2-叔辛基氨基-1,3,5-三嗪。实验考察了氢氧化钠、氢氧化钾、碳酸钠等无机碱和有机碱在上述合成过程中的缚酸作用,确定了较好的缚酸剂为二异丙基乙胺。与传统的氢氧化钠缚酸法相比,无水环境下使用二异丙基乙胺可杜绝三聚氯氰的水解。经实验优化,产物收率达97.0%以上,液相色谱纯度大于99.8%,以此为原料合成光稳定剂944,其收率较氢氧化钠缚酸法提高约5.0%。
The intermediate of HS-944 namely 4,6-dichloro-t-octylamine-1,3,5-triazine was prepared from cyanuric chloride and t-octylamine. The acid-binding behaviors of inorganic bases including sodi- um hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, and organic bases in- cluding t-octylamine, triethylamine and N, N-diisopropylethylamine were studied. The experimental results indicated that N,N-diisopropylethylamine showed better performance in the acid binding effect than other bases. Compared with the traditional method of using sodium hydroxide, N,N-diisopropy- lethylamine was used in anhydrous media and the hydrolysis of cyanuric chloride was eliminate com- pletely. Upon the optimum condition the yield of the product was more than 97.0% with a purity of more than 99.8% measured by HPLC. The yield of HS-944 prepared from the triazineobtained by u- sing N,N-diisopropylethylamine as acid-acceptor was about 5.0% higher than that by using sodium hydroxide.
出处
《精细石油化工》
CAS
CSCD
北大核心
2018年第1期5-8,共4页
Speciality Petrochemicals
