研究采用新型有机溶剂体系合成羟丙甲纤维素邻苯二甲酸酯(HPMCP),并对合成过程进行工艺优化,使之可取代目前工业上普遍使用的冰醋酸反应体系。在新型有机溶剂体系下,以三乙胺为催化剂,羟丙甲纤维素(HPMC)与邻苯二甲酸酐进行酯化反应制备HPMCP;运用单因子变量法考察邻苯二甲酸酐的量、催化剂的量、反应温度及反应时间等对反应程度的影响(以酰化率来衡量)。在新体系下合成出了酰化率及游离酸含量等关键技术指标均符合美国药典要求的HPMCP;考察了各因素对酰化率的影响并得到了最佳反应条件为HPMC∶邻苯二甲酸酐∶三乙胺=1∶1.5∶0.08,65℃下反应7h。
To prepare the hydroxypropyl methylcellulose phthalate(HPMCP)under the new organic solvent system instead of the glacial acetic acid-sodium acetate system and to optimize this process HPMCP was synthesized by hydroxypropyl methylcellulose(HPMC)and phthalic anhydride using triethylamine as a catalyst.Utilizing one-variable method was utilized to study the influence factors on the reaction degree,such as the amount of phthalic anhydride,catalyst,reaction temperature and time.The key properties of synthetic HPMCP,such as degree of acylation and free acid content under the new synthetic system,can meet the requirements of the United States pharmacopoeia.The effects of various factors on the degree of acylation were investigated and the optimum reaction conditions were obtained(HPMC:phthalic anhydride:catalyst=1:1.5:0.08;reaction temperature and time:65℃,7h)