摘要
以取代苯胺为起始原料,与水合氯醛及盐酸羟胺反应生成取代的异亚硝基乙酰苯胺(2a-2e),在浓硫酸作用下环合,经水解后以65.9%-80.3%的总收率得到5位取代的靛红(3a-3d),以39.5%的总收率得到7位取代靛红(3e)。化合物2a-2e的合成作为Sandm eyer法合成取代靛红的关键步骤,对其制备工艺进行优化并确定了最佳反应条件:反应温度为85℃,反应时间为1.5-2.5h。
The substituted aniline as the starting material reacted with chloral hydrate and hydroxylamine hydrochloride to form isonitroacet aniline （2a-2e）, then 2a-2e were cyclized in the concentrated sulfuric acid and hydrolyzed to give isatins （3a-3d） in overall yields of 65.9%-80.3%. The overall yield of 3e was 39.5%. As the key step of Sandmeyer reaction, the conditions of synthesis of 2a- 2e were optimized and the optimal conditions were established as follows： the reaction temperature 85℃, the reaction time 1.5-2.5h.
出处
《渤海大学学报（自然科学版）》
CAS
2009年第3期212-216,共5页
Journal of Bohai University:Natural Science Edition
基金
辽宁省高校重点实验室计划(NO:2008S001)资助项目
