摘要
以间苯二酚为原料,亚硝酸钠-盐酸作为亚硝化试剂,在稳定剂S保护下,通过一锅法即一亚硝化-二亚硝化-水洗-醇洗合成了4,6-二氨基间苯二酚的关键中间体4,6-二亚硝基间苯二酚,并对产物结构进行了红外光谱和近红外光谱分析,考察了反应温度、亚硝化酸钠用量、反应初始时混合溶剂比例和间苯二酚浓度等因素对亚硝化反应的影响。通过正交试验和平行试验对试验条件进行优化后,DNSO产率最高达到86.19%。
One type of 4,6-diaminoresorcinolintermediate(DAR)4,6-dinitrosoresorcinol(DNSO)was successfully synthesized with the resorcinol as raw material and NaNO 2-HCl as nitrosation reagent under the protection of stabilizing agent(S)via one pot method,which was performed by the process of mononitrosation,dinitrosation,water washing and alcohol washing.Its structure was analyzed by FI-IR and NIR,and the effects of reaction temperature,NaNO 2 amount,mixed solvent ratio and the concentration of resorcinol on the yield of DNSO were evaluated.The synthesis conditions were optimized through the orthogonal and the parallel experiments,and the yield of DNSO prepared under the optimized conditions was 86.19%.
作者
李文婧
李露露
李彬央
蔡伟杰
曹亚峰
LI Wenjing;LI Lulu;LI Binyang;CAI Weijie;CAO Yafeng(School of Light Industry and Chemical Engineering,Dalian Polytechnic University,Dalian 116034,China)
出处
《大连工业大学学报》
CAS
北大核心
2023年第3期206-210,共5页
Journal of Dalian Polytechnic University
基金
辽宁省高等学校创新团队及创新人才支持计划(LR2019006)。
