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响应曲面法优化(salen)Co(Ⅲ)(OAc)拆分手性环氧氯丙烷的制备工艺

卢定强1,2,涂清波1,凌岫泉1,王 俊1,梅巧婷1   

  1. 1南京工业大学药学院;2江苏省药物研究所
  • 出版日期:2010-02-05 发布日期:2010-02-05

Optimization via response surface method for (salen)Co(III)(OAc) catalyzed preparation of chiral epichlorohydrin

LU Dingqiang1,2,TU Qingbo1,LING Xiuquan1,WANG Jun1,MEI Qiaoting1   

  1. 1School of Pharmaceutical Sciences,Nanjing University of Technology;2Jiangsu Institute of Materia Medica.
  • Online:2010-02-05 Published:2010-02-05

摘要: 以(salen)Co(Ⅲ)(Oac)为催化剂不对称选择性水解制备手性环氧氯丙烷,采用响应曲面法中的Box-Behnken设计对影响手性环氧氯丙烷光学纯度的4个主要因素(反应温度、水用量、催化剂用量、反应时间)进行优化,建立手性环氧氯丙烷光学纯度的二次多项回归模型方程,并对回归系数进行显著性检验和方差分析。实验结果表明,当反应温度为46.02 ℃、水与环氧氯丙烷的摩尔比为61.10、催化剂与环氧氯丙烷的摩尔比为0.003 937、反应时间为18 h时手性环氧氯丙烷的光学纯度最高,最高光学纯度预测值为102.18%,与实测平均值99.61%基本相符,优化模型有效可靠。

Abstract: The preparation of chiral epichlorohydrin was studied by using asymmetric hydrolysis with (salen)Co(III)(OAc) catalyst. The influences of temperature,catalyst and water amount and reaction time on the optical purity of the produced epichlorohydrin were optimized with Box-Behnken mode of response surface method. A mathematical regression model for the optical purity of chiral epichlorohydrin was established,and the significance test and variance analysis for the regression equation were also analyzed. Results showed that the optimum conditions for the optical purity of chiral epichlorohydrin are:the temperature is 46.02 ℃,the molar ratio of water to epichlorohydrin is 61.10,the molar ratio of catalyst to epichlorohydrin is 0.003937 and the reaction time is 18 h. The predicted optimum optical purity of chiral epichlorohydrin is 102.18%,which is in consistent with the average measured value of 99.61%. Therefore,the regression equation is valid and reliable.

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