Preparation of Coated Cellulose Tri(4 methylbenzoate) Chiral Stationary Phases and Their Application in Enantioseparation

吴海波; 薛兴亚; 李奎永; 周永正

doi:doi：10.3969/j.issn.1004-4957.2019.01.009

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Preparation of Coated Cellulose Tri(4 methylbenzoate) Chiral Stationary Phases and Their Application in Enantioseparation

- Preparation of Coated Cellulose Tri(4 methylbenzoate) Chiral Stationary Phases and Their Application in Enantioseparation
- Vol. 38, Issue 1, Pages: 64-68(2019)
- 作者机构：
  
  1. 浙江华谱新创科技有限公司
  2. 中国科学院大连化学物理研究所分离分析化学重点实验室
- 作者简介：
- 基金信息：
- DOI：doi：10.3969/j.issn.1004-4957.2019.01.009
  CLC：
- Published：2019
- 稿件说明：
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吴海波, 薛兴亚, 李奎永, 周永正. Preparation of Coated Cellulose Tri(4 methylbenzoate) Chiral Stationary Phases and Their Application in Enantioseparation[J]. 2019, 38(1): 64-68.
DOI：

吴海波, 薛兴亚, 李奎永, 周永正. Preparation of Coated Cellulose Tri(4 methylbenzoate) Chiral Stationary Phases and Their Application in Enantioseparation[J]. 2019, 38(1): 64-68. DOI： doi：10.3969/j.issn.1004-4957.2019.01.009.

摘要

以C8硅烷修饰的大孔硅胶作基质，涂覆制备了纤维素-三(4 甲基苯甲酸酯)手性固定相，研究了涂覆溶剂体系对固定相选择性的影响。实验选择氯仿或二氯甲烷作溶剂，分别添加N

N’-二甲基甲酰胺、苯酚、硝基苯、苯甲酸甲酯、苯乙酮涂覆制备了多个手性固定相，并以7种不同结构的手性化合物对固定相进行评价。结果表明，添加剂的种类与添加量对固定相的装柱柱效、保留以及选择性均会产生一定的影响。添加与纤维素酯等质量的苯甲酸甲酯制得的固定相性能较佳，其对于西孟坦中间体和酮咯酸消旋体具有良好的对映体拆分能力，具备工业制备分离的应用潜力。

Abstract

Based on C8 modified macroporous silica

a coated cellulose tri(4 methylbenzoate)(CTMB) chiral stationary phases(CSPs) were prepared.Influences of coating solvent and additive on the enantioselectivity of CSP were investigated.Several CSPs were prepared by coating CTMB in chloroform and dichloromethane

with N

N’ dimethylformamide(DMF)

phenol

nitrobenzene

methyl benzoate and acetophenone as additives

respectively.The enantioselectivities of CSPs were evaluated by using 7 structurally different enantiomers.It was found that column efficiency

retention ability and enantioselectivity of CSPs were affected by the type and amount of additive.The addition of the same amount of methyl benzoate with CTMB would provide the CSPs with better properties

which exhibit a good enantioseparation ability for racemic simendan intermediate and ketorolac

and possess an application potential in industrial preparation and separation.

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