A simple and versatile method for the synthesis of acetals from aldehydes and ketones using bismuth triflate

Acetals are obtained in good yields by treatment of aldehydes and ketones with trialkyl orthoformate and the corresponding alcohol in the presence of 0.1 mol % Bi(OTf)3.4H2O. A simple procedure for the formation of acetals of diaryl ketones has also been developed. The conversion of carbonyl compounds to the corresponding 1,3-dioxolane using ethylene glycol is also catalyzed by Bi(OTf)3.4H2O (1 mol %). Two methods, both of which avoid the use of benzene, have been developed.     

Highly Enantioselective Phenylacetylene Addition to Benzaldehyde Catalyzed by Chiral Tridentate Ligand

Development of new or improved methods for the asymmetric preparation of chiral propargylic alcohols has gained considerable significance during the past years because they are useful building blocks for the synthesis of many biologically active compounds and natural products.[1] A series of chiral tridentate ligands were conveniently synthesized from amino acids with good yields (Scheme 1).[2] A preliminary study of the enantioselective alkynylation of benzaldehyde catalyzed by this chiral tridentate ligand was carried out and up to 83% ee of chiral propargyl alcohols was obtained (Table 1 ). A further investigation of the tridentate ligand is currently underway.     

On noise and fluctuations in a synchronously mode-locked cw laser system

A single-shot and synchronously-scanned streak camera, autocorrelation and noise spectrum analysing techniques are utilized to study the output characteristics of synchronously mode-locked cw lasers. Four main conclusions are drawn: (i) the pulse train from a synchronously-pumped dye laser reveals, besides phase jitter, considerable pulse shape fluctuations; (ii) autocorrelation measurements may be highly misleading when actual pulse shapes are considered; (iii) both the phase jitter and pulse shape fluctuations of the dye laser output are caused by the phase fluctuations of the pumping ion laser pulse train; (iv) the phase jitter of the ion laser proceeds from the fluctuations in the cavity roundtrip time with a characteristic time of about 5 s. Under optimum conditions the rms noise of the dye laser output was 2% and the phase jitter with respect to the rf sine drive of the acousto-optical mode-locker, 30 ps. A qualitative explanation fo the noise properties is given.     

光活性[1]1-联萘酚(BINOL)的不对称合成

由于 1 ,1 -联萘酚 ( BINOL)可作为手性配体或手性催化剂的前体 ,在不对称合成反应中具有广泛的应用 [1,2 ] ,所以如何得到光学纯的 BINOL的研究吸引了许多化学家的注意 .制备光学活性的 BINOL的方法较多 ,但一般效果较好的是用拆分的方法[3,4] .通过 2 -萘酚不对称氧化偶联直接得到 BINOL的方法也有许多报道 [5 ,6 ] ,但结果都不理想 .近来 ,Kocovsky等 [7]用鹰爪金碱作为手性诱导试剂 ,在Cu Cl2 存在下 ,2 -萘酚偶联得 BINOL,其 ee值为 1 0 0 % ,但产率只有 1 4% ,且由于鹰爪金碱价格昂贵 ,限制了该法的应用 .在此基础上 ,我…     

用C60键合硅胶固定相液相色谱分离杯芳烃及杯芳冠醚类化合物

以自合成的C60 键合硅胶液相色谱固定相 ,分别选用3种不同选择性的流动相体系 :异丙醇 -环己烷 ,氯仿 -环己烷和二氯甲烷 -环己烷 ,考察了流动相组成对杯芳烃及杯芳冠醚化合物保留行为和分离选择性的影响。在一定的流动相条件下溶质能得到较好分离。     

Sparse asymptotic minimum variance based bearing estimation algorithm for a single vector hydrophone

For underwater target detection using a single vector hydrophone, sparse asymptotic minimum variance(SAMV) method is used to estimate the target bearing. The SAMV discretizes the entire scanning space and the target bearing is located at the position of the discrete direction. The SAMV algorithm utilizes the sparsity of the spatial signal to improve the estimation performance of the target bearing. Background noise level(BNL) of the bearing estimation of SAMV algorithm is lower than those of the conventional beam forming(CBF)method and minimum variance distortionless response(MVDR) method for different signal noise ratios(SNRs). When the SNR is higher than 0 d B, the direction-finding error of this algorithm is less than 2°. Moreover, the SAMV algorithm has a better dimensional orientation resolution capability. The experimental results show that the SAMV algorithm gives a bearing and time recording map with a lower BNL, which effectively verifies the effectiveness of SAMV algorithm in terms of underwater target detection.     

对-叔丁基杯[8]芳烃键合硅胶制备及其毛细管电色谱性能研究

以γ-(环氧丙氧)丙基键合硅胶为前体,于硅胶表面键合环氧基,在催化剂存在下以杯芳烃钠盐开环制备杯芳烃键合硅胶固定相.该方法反应条件温和,适用性强.将这个新方法首次用于制备对-叔丁基杯[8]芳烃电色谱键合固定相(C8BS),采用加压电色谱初步评价其电色谱性能.研究结果表明,C8BS电渗流(Electrosmoticflow,EOF)较小,但通过控制键合反应及使用压力辅助电色谱可部分弥补上述不足.该固定相的EOF受流动相pH影响小(pH=3-8),同时大环配体屏蔽效应能有效地克服硅羟基引起的碱性化合物拖尾现象,这对电色谱分离具有重要意义.通过分步封尾研究EOF的来源发现,杯芳烃酚羟基对EOF有弱的贡献,这与报道的杯芳烃涂层具有径向电渗流调控能力相一致.     

蒙药新-Ⅱ中微量硒的测定

采用硒 -硫氰酸钾 -罗丹明 B-明胶 - OP体系分光光度法测定蒙药新 - 中微量硒。其含量为 6 .6—7.3μg· g-1 ,回收率为 94 %— 95 %。     

邻硝基乙酰苯胺衍生物的XPS振起伴峰及其价带谱的研究

研究了一组邻硝基乙酰苯胺衍生物的X射线光电子能谱(XPS).观察到硝基的N1s光电子谱有明显分裂,可认为是N1s振起伴峰的反映,而且苯环上的取代基对该振起伴峰强度有影响,按照Pignataro等关于振起伴峰与主峰的能量分离以及分子内电荷转移有关的观点,计算了振起伴峰与主峰的面积比.结果表明,峰间距与面积比的趋势一致.因此二者都可作为分子内电荷转移的粗略估计.