2-吡啶甲醛的制备

2-吡啶甲醛（1）是缓泻药比沙可啶（bisacodyl）的中间体，也是合成有机磷酸酯类解毒药的原料。文献用2-甲基吡啶（2）经N-氧化、酰化、水解后再氧化制得1，但所用氧化剂二氧化硒或四乙酸铅毒性大，易造成环境污染；也可用2经氧化、重排酯化、再氧化、重排、水解而得，步骤长、操作繁琐，收率较低。文献用2与碘混合，得到的复合物在DMSO中加热得到1，总收率35％，但是成本较高，不易放大制备。文献以三氯异氰脲酸（3）氯化2得2-氯甲基吡啶，本研究通过控制2、3的投料比和反应时间，得到收率94．3％的2-二氯甲基吡啶（4）；4再经发烟硫酸水解即可得到1，总收率87．9％。改进后的工艺操作简便，成本较低。反应式如下：     

6,7-二甲氧基-4-芳胺基喹唑啉衍生物的合成与活性筛选

 目的合成6,7-二甲氧基-4-芳胺基喹唑啉衍生物及其抗肿瘤活性筛选。方法以2-氨基-4,5-二甲氧基苯甲酸和醋酸甲脒为原料,合成了10个4位芳胺取代的6,7-二甲氧基喹唑啉衍生物,利用酶联免疫吸附分析法(ELISA)PTK-101试剂盒并对化合物进行活性筛选。结果合成的化合物经IR,¹H-NMR,MS结构表征。初步的生物活性测试表明,这类化合物对表皮生长因子受体(EGFR)酪氨酸激酶有明显的抑制活性。其苯环4′位的取代基变化对活性具有显著影响。结论6,7-二甲氧基-4-芳胺基喹唑啉衍生物可能会在治疗肿瘤特别是非小细胞肺癌方面发挥更大。     

Application of high resolution X-ray emission spectroscopy on the study of Cr ion adsorption by activated carbon

In this work granular activated carbon has been chosen as an absorbent in order to investigate the Cr(VI) reduced by adsorption experiments. Several batch chromium-sorption experiments were carried out using 0.25 g of granular activated carbon in 50 mL aqueous solution containing approximately 70 and 140 mg L^?1 of Cr(VI) and Cr(III), respectively. Cr–Kβ fluorescence spectra of Cr adsorbed in a carbon matrix and Cr reference materials were measured using a high-resolution Johann-type spectrometer. Based on evidence from the Cr–Kb satellite lines, the Cr(VI) reduction process has actually happened during metal adsorption by the activated carbon.     

Mirror system based therapy for autism spectrum disorders

This paper reviews the present theories and empirical research of autisms’ cognitive research and mirror systems and introduces a new hypothesis about the causes of autism spectrum disorders (ASD): autistic mirror neuron dysfunction hypothesis. ASD subjects show obvious lack of the activation of the mirror system during the task of observation or emotional cognition. It is significant to investigate the mirror system for revealing the causes of autism and it is also helpful for developing new ways to diagnose or treat this disorder.     

Estudio prospectivo que compara laparoscopia y cirugía abierta para el tratamiento de cálculos ureterales impactados

Introduction and objectivesTo investigate two ureterolithotomy approaches for treatment of large and impacted upper ureteral stones, we prospectively evaluated the perioperative features of consecutive patients submitted to ureterolithotomy following failure of endourological treatment.MethodsOf the 110 patients included in the study, 34 underwent laparoscopic ureterolithotomy. Patients were divided into three ureterolithotomy subgroups (group A, 76 open procedures; group B, 16 transperitoneoscopies and group C, 19 retroperitoneoscopies). All procedures were performed into a urology residency program.ResultsThe patients’ age, sex, ASA classification and stones characteristics showed no significant difference between the groups. Overall, complication rates and the operation times recorded were similar. One patient had bilateral stones and both sides were managed in a single transperitoneoscopy procedure. Three retroperitoneoscopies were converted to an open surgery due technical difficulties. A prolonged urinary leakage occurred in 3/35 cases (8.5%) where 2 patients were treated by placing a ureteral catheter. Both laparoscopic groups have significantly less analgesia requirements and shorter hospitalization (p < 0.001 and p = 0.003, respectively). All patients were stone-free in the follow-up 1-month visit.ConclusionsTo our knowledge, this is the first prospective comparison of laparoscopic and open ureterolithotomy in a laparoscopic training scenario. Even though these procedures were performed by limited laparoscopic experience urologists, laparoscopy offered significant advantages over traditional open ureterolithotomy, resulting in improved analgesia, shorter hospital stays and similar complication rates.     

转基因西洋参冠瘿组织中人参皂苷类成分的分离鉴定

 目的分离鉴定转基因西洋参冠瘿组织中的化学成分。方法以本研究组转导和培养的西洋参冠瘿组织为实验材料,体积分数为70%乙醇超声提取,硅胶柱色谱分离,用MS,¹H-NMR、¹³C-NMR、HMBC等谱学方法确定结构。结果分离得到5个化合物,分别为20(S)-人参皂苷Rh₁(Ⅰ)、20(S)-人参皂苷Rg₃(Ⅱ)、人参皂苷Re(Ⅲ)、20(S)-达玛烷-3β,6α,12β,20,25-五醇-6-O-α-L-鼠李吡喃糖基-(1→2)-O-β-D-吡喃葡萄糖苷(Ⅳ)和人参皂苷Rg₁(Ⅴ)。结论上述5个成分均为首次从转基因西洋参冠瘿组织培养物中分离得到,化合物Ⅳ为新天然产物。