(±)-6,7-丙酮缩二醇-3-酮-庚酸乙酯合成研究

用对甲苯磺酸-2,3-丙酮缩甘油酯(2)与乙酰乙酸乙酯盐、碳酸二乙酯反应, 制备β-酮酯类衍生物1. 以(±)-1,2-丙酮缩甘油为起始物, 经对甲苯磺酰化、亲核取代、脱羧等反应, 方便、高产率地合成了6,7-丙酮缩二醇-3-酮-庚酸乙酯(1). 试图通过对甲苯磺酸-2,3-丙酮缩甘油酯(2)和乙酰乙酸乙酯双阴离子反应制备6,7-丙酮缩二醇-3-酮-庚酸乙酯(1)未获成功. 所合成的化合物经元素分析, IR, ¹H NMR, ¹³C NMR和MS光谱表征.     

(R)-甘油醛缩丙酮的合成及Wittig反应选择性

D-(R)-甘油醛缩丙酮是近年来研究的很多的一种用来合成一些手性药物和具有光学活性的天然产物的重要前体.用Lew is酸无水ZnC l2作为催化脱水剂,D-甘露醇与丙酮缩合反应合成二异亚丙基缩合物,然后用NaIO4氧化断键制备D-(R)-甘油醛缩丙酮,该方法具有产率高、价廉、环境友好等优点.主要研究了(R)-甘油醛缩丙酮W ittig反应的立体选择性.     

(S)-甘油醛缩丙酮的新合成方法

(S)-甘油醛缩丙酮是一种用来合成一些手性药物和具有光学活性的天然产物的重要前体,本文以L-抗坏血酸为原料,经高压氢化还原、缩合反应、氧化剂氧化等步骤合成(S)-甘油醛缩丙酮.同时考察了不同的反应条件对产品收率的影响.     

S-甘油醛缩丙酮的合成及其Wittig反应

以L-抗坏血酸为原料合成了S-甘油醛缩丙酮;研究了S-甘油醛缩丙酮的Wittig反应立体选择性.     

左旋丙叉甘油醇合成方法的改进

左旋丙叉甘油醇合成方法的改进;L-丝氨酸;合成;左旋丙叉甘油醇;二甲氧基丙烷     

由D-果糖合成新型β-氨基醇

以D-果糖为原料,经羟基保护、选择性脱保护、酯化、叠氮取代、叠氮还原为氨基反应合成了两种新型β-氨基醇,产物结构经13CNMR、1HNMR和MS确证。     

含茂基及双乙酰丙酮缩乙二胺基稀土金属有机配合物的合成及表征

由双乙酰丙酮缩乙二胺与三茂稀土在四氢呋喃溶液中室温下反应,合成了具有通式为（ａｃｅｎ）ＬｎＣｐ（Ｃｐ＝η＾５－Ｃ５Ｈ５,Ｌｎ＝Ｙ,Ｎｄ,Ｔｂ,Ｄｙ,Ｅｒ,Ｙｂ）的６个新稀土金属有机配合物,这些配合物均经元素分析,ＩＲ,ＭＳ和＾１Ｈ ＮＭＲ表征。     

基于D-葡糖胺的手性β-氨基醇的合成

手性氨基醇作为催化剂广泛应用于多种不对称合成反应中。以D-葡糖胺为原料设计合成一系列新型手性β-氨基醇。D-葡糖胺首先与氯甲酸甲酯缩合,再先后经过甲基化、苄叉保护、碱性水解反应,得4,6-O-苄叉基-2-脱氧-2-氨基-α-D-吡喃葡萄糖甲苷,进一步将其通过N-烃化反应或N-磺酰化反应合成得手性β-氨基醇。产物结构经1H NMR,13C NMR和MS表征确证。     

催化氧化法合成缩丙酮—（R）—和（S）—甘油酸

以Ｄ－和Ｌ－酒石酸为原料，合成出高光光纯度的缩丙酮－（Ｒ）－和（Ｓ）－甘油酸（１ａ，１ｂ），总收率分别为３２．８和３４．１％制备的关键步骤为三氯化钌与次氯酸钠对邻二醇结构中Ｃ－Ｃ键的选择性氧化断裂。     

A Practical Synthesis of (S)-(+)-2-(6-methoxyl-2-naphthyl) propionic Acid

a-Arylpropionic acids are an important class of non-steroidal anti-inflammatory agents1,2. The therapeutic efficacy of this class of drugs is well demonstrated by the introduction and extensive use of more than a dozen compounds exemplified by ibuprofen, naproxen, ketoprofen and flurbiprofen etc. However, in recent years the use of enantiomerical pure drugs in chemotherapy is becoming almost mandatory for enhancing specificity of drug action and reducing the toxicity. This awareness led to …     

Synthesis of enantiomericcis-homocaronic acids from (+)-3-carene

The syntheses of the dimethyl ester of (-)-(1R)-cis-homocaronic acid (7 steps, overall yield 43 %) and its antipode, the dimethyl ester of (+)-(1S)-cis-homocaronic acid (5 steps, overall yield 27 %), were performed starting from (+)-3-carene and its derivatives, (+)-4-acetyl-2-carene and (+)-4-acetoxymethyl-2-carene. Oxidative cleavage in the key stages was carried out by ozonization.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 314–318, February, 1995.     

Total Syntheses of (+)-Goniotriol and (+)- 8-Acetylgoniotriol

Two styryl-pyrones, (+)-goniotriol (1) and (+)-8-acetylgoniotriol (2), which are cytotoxic to human turnout cells, were isolated from the ethanolic extracts of the stem bark of Goniothalamus giganteus Hook. F., Thomas (Annonaceae), in addition (+)-goniotriol was also isolated from the leaves and twigs of Goniothalamus     

(+)-(1S,2S,5R)-8-联苯薄荷醇的合成

以(R)-( )-pu legone为起始原料,经1,4-加成,还原两步反应合成了手性辅助试剂( )-(1S,2S,5R)-8-联苯薄荷醇及其差向异构体(-)-(1R,2S,5R)-8-联苯薄荷醇,总产率95%。其结构经1H NMR,13C NMR,IR,MS和X-射线衍射仪表征。     

Synthesis of 1-(1-Aroyl-2-arylvinyl)-2-dicyanomethylen-1,2-dihydropyridines from 2-Chloropyridinium Salts and Unsaturated Nitriles

1-(1-Aroyl-2-arylvinyl)-2-dicyanomethylene-1,2-dihydropyridines are formed from 1-(aroylmethyl)-2-chloropyridinium bromides and arylmethylenemalonitriles in ethanol at room temperature in the presence of a twofold excess of triethylamine. The products are converted into 2-amino-3-aroyl-1-cyanoindolizines on boiling in acetic acid.     

Synthesis and Crystal Structure of (Z)-Ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate

The compound (Z)-ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate 3 has been synthesized by the reaction of ethylacetoacetate 1 and phenylisothiocyanate 2. Its structure has been established by ¹H NMR, ¹³C NMR, infrared, mass spectra, and x-ray crystallography.      

Synthesis, Crystal Structure and Absolute Configuration of (+)-(а-Hydroxybenzyl)phenylphosphinic acid

The title compound (+)-((-hydroxybenzyl)phenylphosphinic acid (C13H13O3P, Mr = 248.20) has been synthesized and characterized by 31P NMR, 1H NMR and elemental analysis. X-ray diffraction analysis at 293(2) K indicates that the compound belongs to monoclinic system, space group C2 with cell parameters: a = 23.560(8), b = 6.947(2), c = 7.854(3) (A。）, β = 91.273(6)°, V = 1285.2(7) (A。）3, Z = 4, Dc = 1.283 g/cm3, F(000) = 520 and ((MoK() = 0.207 mm-1. The number of independent reflections amounts to 1991, of which 1507 are observed reflections. The crystal structure has been determined by direct methods (SHELXL-97). The structure parameters are refined by full-matrix least-squares on F2 to R = 0.0437 and wR = 0.0893. The flack x parameter is - 0.0001. The absolute configuration of the (-carbon in the title compound is S.     

氢氧化铯催化下,二芳基二硒醚对端炔的加成:高选择性合成(Z)-1,2-二芳硒基烯

氢氧化铯催化下,以商业THF作溶剂,端炔与二芳基二硒醚在氮气保护下,25或35℃时反应,立体选择地生成(Z)-1,2-二芳硒基烯.     

Synthesis and Molecular Structure of (E)-1-(Morpholino)-2-(thiomethyl)-2-phenylvinylphosphonate

1 INTRODUCTION Phosphorus-containing vinyl compounds havebeen widely studied due to their versatile physiolo-gical activities and applications in transition metalchemistry, asymmetric catalysis and photorearrange-ment[1～4]. In our previous papers, we have reportedthe syntheses of 2,2,4,5-tetrasubstituted-1,3-dithio-les[5] and 2,5-bis(morpholino)-3,4-bis-(p-chloro-phe-nyl)thiophenes[6] by the reactions of α-thioaroyl-thiofor-mamide with trimethyl phosphite at room tempera-ture and in refl…     

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound.