论文部分内容阅读
以苯胺为原料,经过甲磺酰化、傅克酰基化、异丙胺化和氢化还原得到盐酸索他洛尔产品(Ⅰ),总收率达到75.9%(以苯胺计),化学纯度达到99.8%,最终产物结构通过IR、1HNMR、ESI-MS及元素分析进行表征。该文对甲磺酰化工序的缚酸剂进行研究,确定碳酸氢钠最佳摩尔比为n(碳酸氢钠)∶n(苯胺)=1.1∶1,反应温度为室温,收率为97%;对氢化还原反应的钯炭含量、用量和回收套用进行研究,确定7%钯炭最佳用量为中间体IV投料质量的5%,回收钯炭套用最佳次数为3次。该法合成步骤简便,工艺绿色环保,经济适用,非常适合于产业化大生产。
Using aniline as starting material, sotalol hydrochloride (Ⅰ) was obtained via mesylation, Friedel-Crafts, isopropylamine and hydrogenation reduction. The total yield was 75.9% (aniline) and the chemical purity was 99.8% The final product structure was characterized by IR, 1HNMR, ESI-MS and elemental analysis. In this paper, the acid-binding agent of mesylation was studied and the best molar ratio of sodium bicarbonate was n (sodium bicarbonate): n (aniline) = 1.1:1. The reaction temperature was room temperature and the yield was 97% The optimum amount of 7% palladium on carbon was 5% of the mass of the intermediate IV, and the optimum number of times of palladium-carbon recovery was 3 times. The method has the advantages of simple steps of synthesis, environmental protection and economical application, and is very suitable for industrialized large-scale production.