【摘要】 研究了以庚二酸单乙酯为原料,经酰氯化、傅-克酰基化、水解以及还原得到7-羟基-7-苯基庚酸,再与三甲基氢醌反应制得塞曲司特的工艺.考察了反应物配比、催化剂用量等因素的影响,得较佳工艺参数组合:庚二酸单乙酯∶氯化亚砜=1∶2.2;7-羰基-7-苯基庚酸乙酯∶氢氧化钾=1∶4,碱浓度30%;塞曲司特合成的投料比1∶1.2,催化剂的用量1∶1.2.重点研究了7-羟基-7-苯基庚酸的合成,得正交优化结果:投料比1∶1.2,回流,反应时间6 h.五步反应总收率22.7%.更多还原

【Abstract】 The process for preparation of seratrodast by condensation reaction from 2,3,5-trimethyl hydroquinone and 7-hydroxy-7-phenylheptanoic acid,which was prepared by chlorination,F-C acidylation,hydrolysis and reduction from ethyl pimelate,was studied.The effects of the molar ratio of reactants and the dosage of catalyst were investigated.The optimum process parameters were determined as follows: molar ratio of ethyl pimelate∶SOCl₂=1∶2.2;7-phenyl-7-oxoheptanoate∶KOH=1∶4;Concentration of KOH 30%;7-hydroxy-7-phenylheptanoic acid∶2,3,5-trimethyl hydroquinone=1∶1.2.7-hydroxy-7-phenylheptanoic acid∶BF₃·Et₂O=1∶1.2.The synthesis of 7-hydroxy-7-phenylheptanoic acid was primarily studied,optimum synthesis conditions were obtained as follows: 7-phenyl-7-oxoheptanoic acid∶KBH₄=1∶1.2,reflux,reaction time 6 h.The total yield of seratrodast was 22.7 %.更多还原