CAJ | 학술논문

以磺胺基苯基取代的丙烯酸乙酯为原料,氢氧化钠为碱和催化剂,盐酸羟胺为试剂,通过官能团转化反应,合成了T细胞淋巴瘤的化疗用药贝利司它.采用红外光谱、紫外可见光谱、核磁共振氢谱、质谱、元素分析和熔点测定等技术对产物结构进行了表征.通过单因素变量法探讨了反应物料比、反应温度、碱用量和反应时间对产物产率的影响,得出该反应的最佳工艺条件为:当物料配比n盐酸羟胺:n原料=35:1,碱的用量为0.11mol(当n原料=6.7mmol时),反应温度为0℃,反应时间为60min时,产物贝利司它纯化后产率可达到70%.
이광알기분기취대적병희산을지위원료,경양화납위감화최화제,염산간알위시제,통과관능단전화반응,합성료T세포림파류적화료용약패리사타.채용홍외광보、자외가견광보、핵자공진경보、질보、원소분석화용점측정등기술대산물결구진행료표정.통과단인소변량법탐토료반응물료비、반응온도、감용량화반응시간대산물산솔적영향,득출해반응적최가공예조건위:당물료배비n염산간알:n원료=35:1,감적용량위0.11mol(당n원료=6.7mmol시),반응온도위0℃,반응시간위60min시,산물패리사타순화후산솔가체도70%.
Belinostat was synthesized by functional group conversion from an acrylate derivative to a hydroxamic acid structure by hydroxylamine and base. The structure and purity of the product was characterized by IR, UV-Vis, NMR spectrometry and MS, EA, melting point measurements. And the effects of ratio of reactants, reaction temperature, amount of base and reaction time on the reac-tion yield were also studied. To conclude, the optimized reaction conditions were as followed: 35 equivalent hydroxylamine to start-ing material, 0.11mol base amount based on 6.7mmol starting material scale, reaction temperature 0℃and reaction time 60min. The final yield of belinostat after purification could reach 70%, which was suitable for industrial process development.