七—（2，3，6，—0—烯丙基）—β—环糊精的合成与表征

利用氢氧化钠作催化剂使β-环糊精(简称β-CD)被烯丙基修饰合成了七-(2，3，6-O-烯丙基)-β-环糊精[Heptakis-(2,3,6-O-allyl)-β-CD]。用正交实验法考察了反应温度、反应时间、催化剂用量和修饰剂-烯丙基溴用量等因素对合成目标化合物的影响，得出合成七-(2，3，6-O烯丙基)-β-环糊精的最佳实验条件：n(β-环糊精)：n(烯丙基溴)＝1：86．92，n(催化剂):n(烯丙基溴)＝1：1．052。产物经元素分析，IR和1HNMR表征和确认。     

PPY／PVP催化剂合成11，2，4—三—0酰化红霉素的研究

本文利用4－（1'－四氢吡咯）吡啶（PPY）及聚乙烯吡啶（PVP）复合催化剂催化合成了11,2',4'－三－0酰化红霉素衍生物,与传统方法相比,该法具有简单、快速、收率高等优点。一些影响素及反应机理被讨论,目标物收率为90％以上。     

Crystal Structure of 2—[（P,P—Diphenoxy）phosphono（p—methyl）benzyl]—1,2—

The crystal structure of the title compound 2-[(P, P-Diphenoxy)phosphono(p-methyl)benzyl]-1, 2-benzisoselenazol-3(2H)-one, C27H22NO4PSe, was determined by single crystal X-ray diffraction. It crystallizes in the triclinic system, space group P(No. 2) with Mr=534.41, a=9.761(2), b=10.304(2), c=13.396(3), α=110.97(3), β=107.70(3). γ=90.02(3)°, V=1190(1) 3, Z=2, Dx=1.492 g/cm3, λ=0.71073, μ=1.6596 mm-1 and F(000)=544. The structure was solved by direct methods. The final R factor is 0.068 and Rw is 0.074 for 2500 unique observed reflections [I≥3σ(I)]. The results presented herein indicate that the selenium-containing bicyclic moiety is a coplanar structure and that two adjacent molecules are symmetrically linked to each other forming a dimer through the Se(1c)...O=P(1) bonding interaction with an intermolecular Se(1c)...O distance of 2.797 .     

Crystal Structure of 5—（l—Menthyloxy）—3—chloro—4— Pyrrolidinyl—2（5H0—f

The molecular structure of the title compound 5-(l-menthyloxy)-3-chloro-4-pyrrolidinyl-2(5H)-furanone, C18H28ClNO3(Ⅰ), has been determined by X-ray diffraction at 296(1)K. The crystal is monoclinic with space group P21, a=9.457(3), b=10.413(3), c=9.525(2), β=95.19(2)°, V=934(1) 3, Z=2, Mr=341.88, Dx=1.22 g/cm3, μ=2.15 cm-1, F(000)=368. The final R factor is 0.059, and Rw is 0.065 for 1020 observed reflections with I≥3σ(I). The absolute configuration at C(14) of the acetal carbon was proved to be S, taking into account the known configuration of 1R, 2S, 5R-menthyl moiety. There are three rings in the molecule of this compound: the furanone ring, the pyrrolidine ring and the mentholoxy group ring. The franone ring is connected with the pyrrolidine ring and the mentholoxy ring by N atom and μ2-O bridge atom respectively.     

5—（对羧基苯偶氮）—8—羟基喹啉与铁显色反应的研究及应用

研究了新显色剂 5 (对羧基苯偶氮 ) 8 羟基喹啉 (5 CPAHQ)在阳离子表面活性剂十六烷基三甲基溴化铵 (CTMBA)存在下 ,与铁 (Ⅲ )的显色反应条件。试验结果表明 ,在pH 4 .2～ 5 .6范围内 ,该显色剂可与铁 (Ⅲ )形成 1∶6稳定的红色配合物。在 4 4 8nm波长处配合物的表观摩尔吸光系数为 4 .14× 10 4 L·mol- 1·cm- 1,该法用于力勃隆药片和大黄中铁的测定 ,结果满意     

P—HZSM—5催化剂上合成对异丙基苯酚的研究

研究了在Ｐ－ＨＺＳＭ－５上苯酚与异丙醇烷基化合成对异丙基苯酚（ｐ－ＩＰＰ）的反应,考察了磷含量对催化反应性能的影响,用ＮＨ３－ＴＰＤ和Ｐｙｒ－ＩＲ表征也Ｐ－ＨＺＳＭ－５的表面酸性质 ,结果表明,磷改性ＨＺＳＭ－５可提高ｐ－ＩＰＰ选择性（达９５％）。而降低了苯酚的转化率,并导致酸量减少和酸强度减弱,磷与分子筛的相互作用引起了分子筛脱铝,焙烧温度对活性和选择性均有影响,分子筛在９７３Ｋ、Ｐ－ＨＺＳＭ＿     

环双9对—苯基—对草快）对中性客体的分子识别和分子开关

用AM1及MNDO方法对环双（对－苯基－对草快）与中性客体的配合物进行理论研究，得到稳定化能和配合物相互转换的△△E值；以AM1优化构型为基础，用INDO／SCI方法计算4种配合物光谱，并用AM1方法计算主体与二苯醚衍生物在H^ 存在下的势能曲线，探讨分子开关形成机理。     

用N—苯基—N′—（氨基对苯磺酸钠）硫脲光度法测定微量钯（Ⅱ）

１引言 硫脲类化合物作为显色剂测钯已有报道,氨基硫脲及其衍生物分子中,含有的氮、硫两种原子均可作为电子的给予体,提供电子对与多种金属离子生成金属资合物,因而广泛应用于金属离子的定性、定量分析。本实验室合成的系列氨基硫脲类化合物已成功应用于钯的定量分析。本文研究了新的水溶性试剂Ｎ－苯基－Ｎ’－（氨基对苯磷酸钠）硫脲（ＰＰＴ）与钯（Ⅱ）的显色反应,通过寻找适宜的反应条件,建立了测定微量把（Ⅱ）的新方法。该法灵敏度高、操作简便,且测定结果准确可靠。将该法用于废催化剂中把的测定,所得结果令人满意。２实验…     

2—对甲氧基苯基—4—苯基—1，5—苯并硫氮杂草Zhuo—α—（N—噁唑烷酮基）—β—内酰胺的反相高效液相色谱法测定

建立了一种测定 2 -对甲氧基苯基 -4 -苯基 -1,5 -苯并硫氮杂(艹卓) -α -(N -噁唑烷酮基) -β -内酰胺 (MPPBOL)的反相高效液相色谱法,色谱柱为 Hypersil ODS2(4.6 mm× 250 mm,5 μ m),流动相为 CH3CN-CH2Cl2-H2O(体积比 70∶ 0.5∶ 30),检测波长 240 nm; MPPBOL在 0.1～ 10 mg范围内,峰面积与待测物质的质量呈良好的线性关系,相关系数为 0.999 4,相对标准偏差 3.4%(m=1.0 mg,n=6),回收率在 97%～ 103%之间.     

Crystal Structure of cis—2—[P,P—Diethoxy） phosphono（m—nitro）benzyloxy]

The crystal structure of the title compound cis-2-[(P, P-Diethoxy)phosphono(m-nitro)benzyloxy]-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide, C22H29NO8P2S, was determined by single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with Mr=529.49, a=9.888(2), b=20.831(4), c=12.797(3) , β=94.42(3)°, V=2628(1) 3, Z=4, Dx=1.338 g/cm3, λ=0.71073, μ=0.2796 mm-1 and F(000)=556. The structure was solved by direct methods. The final R factor is 0.052 and Rw is 0.057 for 1793 unique observed reflections [I≥3σ(I)]. A cis-configuration and a preferred chair conformation for the molecule have been established by X-ray diffraction analysis. The results presented also give a good explanation to the correlation between the configurational assignments and the regularity in the chemical shifts of C4-H and 31P NMR.