ω-氯甲基长叶烯的合成及其抑菌活性

以ω-羟甲基长叶烯（Ⅰb）为原料,经过卤代反应,合成了ω-氯甲基长叶烯（Ⅰc）,产物经FTIR、1HNMR、（13）CNMR和HRMS等进行了结构表征。考察了反应温度、反应物配比[n（SOCl_2）∶n（Ⅰb）]和反应时间对卤代反应的影响。结果表明：在较佳的反应条件[反应温度85℃,n（SOCl_2）/n（Ⅰb）=1.10,反应时间6 h]下,Ⅰc产率达94.2%。初步的抑菌活性实验结果表明：Ⅰc对金黄色葡萄球菌、肺炎克雷伯氏菌和白色念珠菌的生长具有明显的抑制作用,其最低抑菌质量浓度分别为31.3、62.5和125 mg/L,且远小于长叶烯的最低抑菌质量浓度（〉500 mg/L）。运用密度泛函理论（DFT）,采用B3LYP/6-31G方法对Ⅰc和长叶烯进行几何结构优化,结果表明,Ⅰc抑菌活性高于长叶烯,与Ⅰc的前线轨道能隙（0.063 a.u）比长叶烯（0.256 a.u）小有关。

Synthesis, Crystal Structure, and Herbicidal Activity of(3R,4R)-4,7,7-Trimethyl-6-oxabicyclo[3.2.1]octane-3,4-diol Mono-fatty Acid Esters

Four mono-fatty acid esters(Ia～d) were synthesized via the esterification of(3R,4R)-4,7,7-trimethyl-6-oxabicyclo[3.2.1]octane-3,4-diol(I) with fatty acid chlorides(CH_3(CH_2)_nCOCl, n = 0, 2, 4, 6) and structurally characterized by means of H RMS, IR, ~1 H-NMR, ^(13)C-NMR and X-ray diffraction. Compounds Ia～d all belong to monoclinic system, P2_1/c space group. Intermolecular O(2)–H(2)···O(1) hydrogen bonds, intramolecular O(2)–H(2)···O(3) hydrogen bonds and van der Waals' interaction between fatty acid ester groups link each of the mono-fatty acid ester molecules into a bilayer structure similar to liposome with the exposed hydrophobic moiety and the sandwiched lipophilic moiety. Especially, compounds Ia～d could be dissoluble or scattered in aqueous solution and showed hydrophilic/lipophilic property-dependent herbicidal activity against the dicotyledon plant rape(Brassica campestris) and the monocotyledon plant barnyard grass(Echinochloa crus galli). At the concentration of 10 mmol·L^(-1), the inhibition rates of compounds Ia～d against the root growth of rape are 31.9, 90.8, 99.5 and 100%, respectively and the inhibition rates against the shoot elongation of barnyard grass are 19.3, 50.0, 80.2 and 100%, respectively.

有机化学实验“演讲评”综合考核模式研究与实践

有机化学实验是高等学校化学相关专业重要的一门实践课程,传统的教学与考核方式多为动手操作或笔试考核为主,方式单一,不利于学生综合能力的培养与提升。为拓宽教学途径,有效提高有机化学实验的教学质量,采用"演讲评"综合考核模式应用于该课程的教学环节中,该模式对调动学生学习的积极性与主动性,巩固专业知识、提高专业技能素质、培养创新精神与团队协作意识有良好的助推作用。

Synthesis, Crystal Structure and Antimicrobial Activity of(E)-2-(2-(4,8,8-Trimethyldecahydro-1,4-methanoazulen-9-ylidene)ethyl)benzo[d]isothiazol-3(2H)-one

The title compound(E)-2-(2-(4,8,8-trimethyldecahydro-1,4-methanoazulen-9-ylidene)ethyl)benzo[d]isothiazol-3(2H)-one(Ic)was synthesized from longifolene and 1,2-benzoisothiazolinone(short as BIT)through Prins,halogenation and nitro-alkylation reaction and structurally identified by means of HRMS,IR,1H-NMR,13C-NMR and single-crystal X-ray diffraction.The crystal of compound Ic is of bi-molecular structure and belongs to orthorhombic system,P212121 space group with a=7.5715(7),b=16.8824(9),c=31.1926(14)?,V=3987.2(5)A^3,Mr=367.53,Dc=1.225 mg/m^3,Z=8,μ=0.174 mm^–1 and F(000)=1584.A total of 17045 reflections were collected,of which 7306 were unique(Rint=0.0566).The structure was refined to R=0.0967 and wR=0.1998 for 7306 observed reflections withⅠ>2σ(Ⅰ).1D chain along the a-axis is formed by two types ofπ-πinteractions between benzene rings from adjacent molecules.Especially,compound Ic shows improved solubility in nonpolar organic solvents and higher antimicrobial activity than longifolene and BIT against bacteria and fungi.The minimum inhibition concentration(MIC)of Ic against two Gram-positive bacteria(S.aureus and B.subtili),two Gram-negative bacteria(E.coli and K.pneumoniae)and three fungi(C.albicans,C.tropicalis and A.niger)are 0.242,0.242,15.6,15.6,1.95,1.95 and 1.95μg/mL,respectively.

丙烯酰胺与马来松香丙烯酸酯防腐共聚膜的制备

以丙烯酰胺(AM)为单体、马来松香丙烯酸乙二醇酯(EGMRA)为交联剂在6063铝合金上热合成了一种共聚膜。采用傅里叶变换红外光谱、扫描电镜分别对共聚膜的结构及形貌进行了研究。结果表明在6063铝合金上已合成了AM与EGMRA的共聚膜。在NaCl质量分数3.5%的溶液中测试了不同EGMRA浓度下合成的聚合膜的电化学性能,结果表明,EGMRA的浓度为0.04~0.06 mol./L时,共聚膜显示出较高的防腐蚀性能。制备的共聚膜对铝合金的保护效率达95.2%。同时也比较了单独的AM聚合膜与共聚膜的防腐蚀性能,结果表明共聚膜能更高效地保护铝合金。