新马兜铃内酯的晶体结构

从绵毛马兜铃的根茎中分离出一种新的倍半萜内酯, 它的分子式由高分辨质谱数据确定为C~1~5H~2~0O~2, 它的结构用单晶X射线衍射法测定, 晶体属三斜晶系, 空间群为P1, a=0.6275(3)nm, b=0.8057(4)nm, c=1.3622(6)nm; α=88.78(4)°,β=91.44(4)°, γ=105.20(4)°; Z=2.3107。     

钯催化α-炔醇立体专一合成α-（Z）-氯亚甲基-β-内酯

首次在一氧化碳存在下，以仲丁醇和苯为混合反应溶剂，氯化钯和氯化铜为催 化体系催化α-炔醇羰基化，立体专一合成α-（Z）-氯亚甲基-β-内酯环。     

MOLECULAR ENGINEERING STUDIES ON NONTHROMBOGENIC BIOMATERIALS——A NOVEL CLASS OF NONTHROMBOGENIC BIOMATERIALS WITH ZWITTERIONIC STRUCTURE OF CARBOXYBETAINES

N,N-dimethyl-N-methacryloyloxyethyl-N-carboxyethyl ammonium (DMMCA) was graft-copolymerized onto the surface of segmented poly(ether urethane) (SPEU) and PE film. The carboxybetaine structure on SPEU and PE film surfaces was confirmed by ATR-FTIR, XPS and water contact angle measurements. Through the experiments with platelet adhesion and protein adhesion assay in vitro, the two materials studied, including poly-DMMCA gel, all show excellent nonthrombogenicity. This confirms once again that the zwitterionic molecular structure on the surfaces of materials is essential for improving their nonthrombogenicity and biocompatibility.     

I_2-KIO_3-AcOH-H_2O体系氧化3,5-环-24S-乙基-胆甾-22烯-6-酮反应的研究

油莱甾醇内酯(Brassinolide)(1)是一种高效的植物生长激素,其生理活性与侧链中C_(22)、C_(23)的构型密切相关。当C_(22)、C_(23)为S、S构型时,其活性仅为1的十分之一。在1的     

N－甲基吡咯烷酮、α－吡咯烷酮合成物系气相色谱分析

 This paper describes a GC analytical method in the synthes is of N-methyl pyrrolidone of a-pyrrolidone.This procedure was performed with a column packed with 6%OV-17/silanized 101 support and FID detec-tor. Calibration factors and detection conditions are given,The coefficients of variation of NMP and a-P were0.6%and 0.5%respectively. The relative errors of all the components were not more than±3.0%,Thequantitative analysis is fast,simple and accurate.     

Sesquiterpene Lactone Glycosides from Carpesium macrocephalum

Two new sesquiterpene lactone glycosides were isolated from the seeds of Carpesium meacrocephalum. Their structures were elucidated as 2α-O-β-D-glucopyranosy-5α,11αH-eudesma-4(15)-en-12,8β-olide and 2α-O-β-D-glucopyranosy-5αH-eudesma-4(15),11(13)-dien-12,8β-olide by spectral methods (HRMS,1D and 2D NMR).     

螺[1-氯-4-l-孟氧基-5-氧杂-6-氧代双环[3·1·0]己烷-2,3'-(4'-吗啉基-5'-l-孟氧基丁内酯)]合丙酮的合成及晶体结构

利用新手性源,5-(l-孟氧基)-3-氯-2(5H)-呋喃酮4与亲核试剂吗啉通过串联不对称双Michael加成/分子内亲核取代反应合成了一般方法难以得到的含有多个手性中心的螺-环丙烷双内酯化合物C32H50O7NCl.其单晶为C32H50O7NCl(OC3H6)0.5,正交晶系, 空间群为P212121, 晶胞参数a = 17.149(3), b = 20.384(4), c = 10.831(2) , V = 3786.1(12) 3, Z = 4, Dc = 1.097 g/cm3, F(000) = 1352, μ= 0.144 mm-1; 射线类型为MoK?( = 0.71073 ?, 偏离因子R = 0.0755, wR = 0.1956, 独立衍射点3710个, 其中可观测点数2318个.分子中共有六个环, 12个手性中心, 3个六元环呈椅式构象, 两个五员内酯环呈信封式构象, 并分别与环丙烷形成[2.4]螺环和 [3.1.0] 稠环, 4个新生成的手性中心的绝对构型为C(3)(S), C(4)(S), C(5)(R), C(8)(R).     

1^H、7^Li、23^Na、133^Cs NMR研究含氮大环醚双内酯和大环胺双内酰胺的配合性能

本文报道~1H、~7Li、~(23)Na、~(133)Cs NMR测定N,N’-二羧甲基大环醚双内酯(1—4)和大环胺双内酰胺(5),N-对甲苯磺酰基大环醚双内酯(6,7),4’-丹磺酰氨基苯并-18-冠-6(8)与Li~+、Na~+、K~+、Cs~+、Cd~(2+)和Pb~(2+)金属离子的配位作用,并以非线性最小二乘法拟合计算了配合物的形成常数;同时,发展了一种用~(133)Cs NMR测量冠醚和碘离子竞争配合Cs~+的配合物形成常数的新技术.     

Baeyer-Villiger oxidation of ketones with hydrogen peroxide catalyzed by Sn-aniline complex

Sn-aniline complex was prepared by a simple procedure.Cyclic and acyclic ketones were oxidized into lactones or esters with very high selectivity and yield with 30% hydrogen peroxide in the presence of Sn-aniline complex.     

抗霉素合成概览

抗霉素(antimycin)是一大类具有九元环双内酯的天然抗生素, 最早发现于20世纪40年代末. 在随后的50多年中不断地有新的成员被发现, 到目前为止已多达26个. 这类化合物的结构主要是通过抗霉素A_3b来确定的, 所以合成工作也是围绕该成员展开的. 对文献中已有报道的合成工作加以综述, 对各方法的主要优缺点也进行了简要的分析.