共查询到20条相似文献,搜索用时 31 毫秒
1.
以醋酸酐为溶剂, 将9, 9-二(4-羟基苯基)呫吨与浓硝酸在15 ℃左右发生硝化反应1.5 h, 形成中间体-9, 9-二(3-硝基-4-羟基苯基)呫吨, 产率为88.5%;继而以Pd/C 为催化剂, 80%的水合肼为还原剂, 在乙醇和1, 4-二氧六环混合溶剂中, 于70 ℃将中间体进行还原反应10 h, 得到目标产物9, 9-二(3-氨基-4-羟基苯基)呫吨, 产率为90.8%, 两步反应总收率为80.4%。 中间体与目标化合物经NMR、FTIR和元素分析等确定了它们的结构。 相似文献
2.
A. V. Varlamov A. N. Levov A. A. Fomichev A. é. Aliev S. Dush Santush A. A. Ustenko I. L. Pashentseva N. S. Prostatkov 《Chemistry of Heterocyclic Compounds》1991,27(2):173-177
Nitration of 9-benzylidene-4-azafluorene with acetyl nitrate leads to the formation of its 9--nitrobenzylidene derivative; reduction of the latter gives the corresponding enamine and oxime. Reaction of 4-azafluorene with ethyl benzoate and ethyl formate gives the hydroxybenzylidene and hydroxymethylene derivatives, which upon condensation with amines generate the corresponding enamines. Reduction of 9-formylazafluorene oxime gives 9-aminomethyleneazafluorene. All of the newly synthesized compounds were isolated in the form of mixtures of their Z- and E-isomers, and their structures were established using PMR spectroscopy.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 212–217, February, 1991. 相似文献
3.
4.
5.
《合成通讯》2013,43(22):3413-3417
ABSTRACT Conditions for efficient resolution of (±)-1-(9-anthryl)ethylamine ((±)-1) by fractional crystallization of its salts with (S)-(+)-mandelic acid (2) are reported. When crystallization was performed by fast addition of chloroform solution of an equivalent of (±)-1 to the hot chloroform solution of (+)-2, crystals of mandelate of (+)-1-(9-anthryl)ethylamine ((R,S)-3) are collected in 56% yield. (R)-(+)-1 (98.6% e.e.) is isolated by extraction from bicarbonate solution of mandelate salt. Ulterior collection of four crops afforded (R,S)-3 with 71.5% cumulative yield and >98% e.e. of (+)-1 in a any single crop. With only 0.5 equivalents of (+)-2 crystallization afforded (R,S)-3 in 47.4% yield and (+)-1 with 98.1% e.e. 相似文献
6.
P. I. Zakharov N. M. Kolyadina N. S. Prostakov Mazhed Gassan N. I. Golovtsov 《Chemistry of Heterocyclic Compounds》2000,36(11):1300-1305
A mass-spectral study was carried out on the behavior of the Z- and E-isomers of 9-picolylideneazafluorenes. A possible mechanism for the elimination of a hydrogen atom from the M+ ion of the Z- and E-isomers of 1(4)-azafluorene derivatives was examined. Mass spectrometry permitted a distinction between compounds isomeric relative to the position of the nitrogen atom in the azafluorene fragments and also the Z- and E-isomers of picolylidene derivatives of 1- and 4-azafluorenes possessing - and -pyridyl substituents. 相似文献
7.
以高藜芦胺为起始原料,经N-磺酰化反应制得高藜芦磺酰胺(2);2分别与芳乙烯甲醚经对甲苯磺酸催化的Pictet-Spengler反应后用金属钠脱除Ts基团合成了(±)-norlaudanosine(5a)和(±)-O,O-dimethylcoclaurine(5b);使用半量拆分法,以N-乙酰-L-苯丙氨酸为拆分剂,制得(S)-(-)-5a和(S)-(-)-5b,其结构经1H NMR,13C NMR,IR,MS和HR-ESI-MS确证。 相似文献
8.
本文提出了一个改进的合成两个光学异构纯的94S)-1- 烯-8, 9-二醇的方法,其优点是简便、有效, 适于克量级制备。 相似文献
9.
本文提出了一个改进的合成两个光学异构纯的94S)-1- 烯-8, 9-二醇的方法,其优点是简便、有效, 适于克量级制备。 相似文献
10.
11.
12.
Li WL Romanescu C Galeev TR Piazza ZA Boldyrev AI Wang LS 《Journal of the American Chemical Society》2012,134(1):165-168
We report the observation of two transition-metal-centered nine-atom boron rings, Rh?B(9)(-) and Ir?B(9)(-). These two doped-boron clusters are produced in a laser-vaporization supersonic molecular beam and characterized by photoelectron spectroscopy and ab initio calculations. Large HOMO-LUMO gaps are observed in the anion photoelectron spectra, suggesting that neutral Rh?B(9) and Ir?B(9) are highly stable, closed shell species. Theoretical calculations show that Rh?B(9) and Ir?B(9) are of D(9h) symmetry. Chemical bonding analyses reveal that these complexes are doubly aromatic, each with six completely delocalized π and σ electrons, which describe the bonding between the central metal atom and the boron ring. This work establishes firmly the metal-doped B rings as a new class of novel aromatic molecular wheels. 相似文献
13.
14.
反式9, 10-二氢-9, 10-二苯基-9, 10-菲二醇包结性能的研究 总被引:5,自引:0,他引:5
合成了一种具有螯形结构的反式-9, 10-二氢-9, 10-二苯基-9,10-菲二醇(1)作为主体分子。它能与许多有机小分子化合物, 诸如DMF, DMSO, 吡啶, 哌啶, 喹啉, 异喹啉等形成包结化合物。本文还报道了这些包结化合物的IR, 粉末XRD的表征, 用^1H NMR谱测定了它们的分子摩尔比。DMF包结物的单晶四圆X衍射结果表明主体分子1与客体分子形成的包结物为配位笼状包合物。 相似文献
15.
The title compound (9S)-2'-O-benzoyl-9,11-[carbonylbis(oxy)]-9-deoxo-5-O-(-D-desosaminyl)-12,21-anhydro-9-hydroxyerythronolide A 1 was synthesized. The crystal structure of the acetone solvate of 1, C37H55NO11·C3H6O, was determined by single-crystal X-ray diffraction analysis. It belongs to monoclinic system, space group P21 with a = 14.4691(10), b = 8.2626(6), c = 17.5990(11) A, β = 94.167(1)°, V = 2098.4(2)A3, M,= 748, Z = 2, De= 1.184 g/cm3,μ = 0.087 mm-1, F(000) = 808, S = 1.026, R= 0.0542 and wR = 0.1322 for 3331 observed reflections (I > 2σ(Ⅰ)). In the solid state, molecules of 1 are linked into spirals along the b axis by O(25)-H(25)…O(29) intermolecular hydrogen bond. 相似文献
16.
Four exotic chiral organocatalysts, 9-amino-(9-deoxy) cinchona alkaloids with (8S, 9R) and (8R, 9S)- configurations, were conveniently synthesized for the first time in 27-72% total yields through two conversions of configuration at the 9-stereogenic centers of commercially available cinchona alkaloids. 相似文献
17.
《Tetrahedron letters》1986,27(38):4629-4632
Short practical syntheses are reported of the title lignans (9a) , (9c) , (13a), and (13b). 相似文献
18.
Pawluć P Franczyk A Walkowiak J Hreczycho G Kubicki M Marciniec B 《Organic letters》2011,13(8):1976-1979
The one-pot synthesis of (E)-9-(2-iodovinyl)-9H-carbazole via sequential ruthenium-catalyzed silylative coupling of N-vinylcarbazole with vinyltrimethylsilane and iododesilylation is reported. Its use as a new building block in the palladium-catalyzed Sonogashira and Suzuki-Miyaura coupling reactions to yield new carbazole-containing (E)-but-1-en-3-ynes and (E,E)-buta-1,3-dienes is demonstrated. 相似文献
19.
20.
The title compound (9S)-2′-O-benzoyl-9,11-[carbonylbis(oxy)]-9-deoxo-5-O-(-D-desosaminyl)-12,21-anhydro-9-hydroxyerythronolide A 1 was synthesized. The crystal structure of the acetone solvate of 1, C37H55NO11·C3H6O, was determined by single-crystal X-ray diffraction analysis. It belongs to monoclinic system, space group P21 with a = 14.4691(10), b = 8.2626(6), c = 17.5990(11) , β = 94.167(1)°, V = 2098.4(2)3, Mr = 748, Z = 2, Dc = 1.184 g/cm3, μ = 0.087 mm-1, F(000) = 808, S = 1.026, R = 0.0542 and wR = 0.1322 for 3331 observed reflections (I > 2σ(I)). In the solid state, molecules of 1 are linked into spirals along the b axis by O(25)- H(25)···O(29) intermolecular hydrogen bond. 相似文献