羧酸甲乙酯中羰基17O-NMR化学位移研究

提出了计算羧酸甲乙酯中羰基¹⁷O-NMR化学位移的公式：δ_cal（¹⁷O）=360.0+Δα+Δβ+Δγ,通过线性回归法确定了22种取代基参数.经回归检验表明该公式计算结果置信度为99.5%,与实验值的偏差Δδ在5.0以内的羰基¹⁷O-NMR化学位移计算值~100%.     

Comments concerning ‘study of molecular interaction in binary liquid mixtures of ethyl acetoacetate with chloroform and dimethylsulphoxide using excess acoustic parameters and spectroscopic methods’

The measured excess molar volume data in the recently published paper for the binary chloroform + ethyl acetoacetate system are shown to differ significantly from previously published data. Excess adiabatic compressibilities reported in the paper are shown to be calculated from an incorrect thermodynamic expression.     

A novel organocatalytic multi-component reaction: an efficient synthesis of polysubstituted pyrano-fused spirooxindoles

A practical, simple, and efficient method for the synthesis of pyrano-fused spirooxindoles via an organocatalytic three-component reaction of isatins, malononitrile, and dialkyl acetylenedicarboxylate in the presence of 3,4-dimethylaniline as an organocatalyst in ethanol is reported. The structures of these products are confirmed by IR, ¹H NMR and ¹³C NMR spectroscopy, mass spectrometry, and single-crystal X-ray diffraction studies.     

Spectroscopic studies and crystal structure of a dimeric Zn(II) complex with diethyl (pyridin-2-ylmethyl)phosphate

The crystal structure of [Zn₂(2-pmOpe)₂Cl₄] (2-pmOpe?=?diethyl (pyridin-2-ylmethyl)phosphate) was determined by X-ray-diffraction method. The compound was also characterized by IR, far-IR, 1H, and ³¹P NMR spectroscopy. In this compound, 2-pmOpe is a bidentate N,O-bridging ligand and Zn(II) are slightly distorted tetrahedral ZnNOCl₂. Zn(II) ions are doubly bridged by the 2-pmOpe ligands, resulting in a dinuclear species. The structure is stabilized by intermolecular C–H?···?O and C–H?···?Cl hydrogen bonds. The spectral properties are in agreement with the structural data.     

One-Pot Stereoselective Synthesis of Alkyl (Z)-2-[4-Oxo-3-phenyl-2-(phenylimino)-1,3-thiazolan-5-yliden]acetates from Acetylenic Esters and N,N′ -Diphenylthiourea

N, N′ -diphenylthiourea reacts with dialkyl acetylenedicarboxylates in acetone to form 1:1 adducts, which undergo a cyclization reaction to produce alkyl (Z)-2-[4-oxo-3-phenyl-2-(phenylimino)-1,3-thiazolan-5-yliden]acetates in fairly good yields. NMR spectra indicated that the reaction is completely stereoselective.     

The Synthesis of Amino Acid Methyl Ester 5′-Phosphoamidates of Protected Uridine

In this article, we used the Atherton–Todd reaction to synthesize amino acid methyl ester 5′-phosphoamidates of uridine as prodrugs. Their structures were confirmed by ¹H NMR, ³¹P NMR, ¹³C NMR, IR, and mass spectrometry.

Supplemental materials are available for this article. Go to the publisher′s online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Synthesis of Novel 1,2,3,4-Tetrahydrocarbazole Derivatives of Biological Interest

2-Cyano-N-(tetrahydrocarbazole)acetamide (1) was utilized for the synthesis of several new arylazocarbazole derivatives (2a–e). Compound (1) reacted with phenyl isothiocyanate to yield the corresponding non-isolable intermediate (3), which gave, upon treatment with dilute hydrochloric acid, thiocarbamoyl derivative (4). Compound (3) reacted with chloroacetone, chloroacetic acid, chloroacetyl chloride, ethyl bromoacetate, and phenacyl bromide to afford thiazolone derivatives (6), (8), and (10), respectively. Compound (1) was heated in the presence of pyridine and/or hydrazine hydrate and/or isatine to give the corresponding tetrahydrocarbazole derivatives (13), (14), and (18), respectively.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Anti‐static Agent Containing Zinc Oxide and its Modification for PA6 Fiber

A new anti‐static agent was synthesized from zinc oxide‐adipic acid‐polyethylene glycol and caprolactam by three‐step reactions. The antistatic agent (called poly(ether ester amide zinc oxide) or PEEAZ) was analyzed by IR and DSC. The results showed that zinc oxide existed in the main chain of PEEAZ. The glass temperature and melt temperature of poly(ether ester amide zinc oxide) (referred to as PEEAZ in the following) decreased with increasing poly(ether ester zinc oxide) increasing in PEEAZ. Antistatic PA6 fiber was obtained by adding PEEAZ 2–8% (wt/wt) to PA6 during blend spinning. The specific resistance and the static half‐value period of PA6 fiber was less than 10⁹Ω · cm and 60 sec, respectively. Excellent antistatic property remained after being washed 30 times.     

Hypervalent Iodine in Synthesis XXXIV: Palladium-Catalyzed Coupling Reaction of o-Hydroxyarylaldehydes with Hypervalent Iodonium Salts Via Cleavage of the Aldehyde C-H Bond

A novel way of preparation for o-hydroxyarylketones with mild conditions and good yields by palladium-catalyzed coupling reaction of o-hydroxyarylaldehydes with hypervalent iodonium salts via the cleavage of the aldehyde C-H bond has been reported.     

One‐Pot,High‐Yielding Synthesis of Novel Dihydrothiazolo[3,2‐a]pyrimidinones

Reaction between 6‐(un)substituted‐2‐thiouracils and E‐ethyl 4‐bromocrotonate under basic conditions at room temperature is an easy, mild, high‐yielding, and regioselective method for the preparation of 7‐(un)substituted dihydrothiazolo[3,2‐a]pyrimidinone derivatives.