摘要
通过重氮偶合、还原环化和酯化反应合成了5-氯-2-[2-羟基-3-叔丁基-5-(3-丙酸甲酯基)苯基]-2H-苯并三唑,并进行了工业放大实验,收率53.0%~55.O%。偶合反应时,以十二烷基苯磺酸钠为乳化试剂,pH=5~8,收率为73.7%;采用n(偶合物):n(保险粉):n(NaOH)=1.0:3.5:15.8进行还原反应,收率81.0%。用MS和。HNMR谱图表征了产物的结构,测定了产物的紫外吸收和透光率。
5-Chloro 2 [ 2-hydroxy-3-tert-butyl-5 -(2-methoxycarbonylethyl) phenyl]-2H-benzotriazole was synthesized through four steps including diazotization, coupling, hydrogenation and esterifica- tion. The yield in laboratory and the scaled up process was 56.2% and 53.0%- 55.0%, respectively.In the process of coupling, at pH=5 -8 with sodium dodecyl benzenesulfonate as emulsification, the yield was 73.7%. In the process of hydrogenation, with the optimal ratio of n(dye) : n(rongalite) : n (sodium hydroxide) =1.0 : 3.5 : 15.8, the yield was 81.0%. The product was characterized by MS and ^1 H NMR. The abilities of UV-absorption and permeating light of the product were measured.
出处
《精细石油化工》
CAS
CSCD
北大核心
2006年第2期31-34,共4页
Speciality Petrochemicals
关键词
苯并三唑
紫外线吸收剂
重氮偶合
还原
酯化
benzotriazole
ultraviolet light absorber
diazotization-coupling
hydrogenation
esterification