Emerging solvent-induced homochirality by the confinement of achiral molecules against a solid surface
Emerging solvent-induced homochirality by the confinement of achiral molecules against a solid surface
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DOI：
10.1002/anie.200800255
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发表时间：
2008-01-01
影响因子：
16.6
通讯作者：
De Feyter, Steven
中科院分区：
文献类型：
--
作者：
Katsonis, Nathalie;Xu, Hong;De Feyter, Steven
起始材料是从Aldrich或Acros购买的，并在收到时使用。洋葱假单胞菌的脂肪酶是从福尔卡中获得的。所有溶剂在使用前都是试剂级的，并干燥和蒸馏。所有水溶液的制备均使用脱盐水。柱层析采用硅胶(Aldrich 60,230-400目)。硅胶60/硅藻土F254色谱柱。在VARIAN VXR300(1H为299.97兆赫，13C为75.48兆赫兹)或瓦里安AMX400型(1H为399.93兆赫，13C为100.59兆赫)光谱仪上记录了CDCl3的1H和13C核磁共振谱。化学位移以相对于残留溶剂峰的值(Ppm)为单位(CHCl3，1H=7.24，13C=77.0)。碳指认是基于APT 13C实验。分裂模式如下：S(单胞胎)、d(双胞胎)、t(三胞胎)、q(四胞胎)、m(多胞胎)、br(宽体)。在JEOL JMS-600h上记录了质谱图。高效液相色谱分析在岛津高效液相色谱系统上进行，该系统配备了两个LC-10AD VP溶剂输送系统、DGU-14A脱气器、sIL-10AD VP自动进样器、SPD-M10A VP二极管阵列检测器、CTO-10A VP柱烤箱和SCL-10A VP系统控制器，分别使用每种化合物指示的柱。
Starting materials were purchased from Aldrich or Acros and used as received. Lipase from Pseudomonas cepacia was obtained from Fluka. All solvents were reagent grade and dried and distilled prior to use. Demineralized water was used in the preparation of all aqueous solutions. Column chromatography was performed on silica gel (Aldrich 60, 230-400 mesh). TLC was performed on silica gel 60/Kieselguhr F254. 1H and 13C NMR spectra were recorded on a Varian VXR300 (299.97 MHz for 1H, 75.48 MHz for 13C) or a Varian AMX400 (399.93 MHz for 1H, 100.59 MHz for 13C) spectrometer in CDCl3. Chemical shifts are reported in values (ppm) relative to the residual solvent peak (CHCl3, 1H= 7.24, 13C= 77.0). Carbon assignments are based on APT 13C experiments. Splitting patterns are indicated as follows: s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), br (broad). Mass spectra (HRMS) were recorded on a Jeol JMS-600H. HPLC analysis was performed on a Shimadzu HPLC system equipped with two LC-10AD vp solvent delivery systems, a DGU-14A degasser, a SIL-10AD vp auto injector, an SPD-M10A vp diode array detector, a CTO-10A vp column oven, and an SCL-10A vp system controller using the columns indicated for each compound separately.