Synthesis, Crystal Structure and Antibacterial Activities of 3-[（2-Hydroxy-4-diethylamino-phenyl）methylenehydrazinocarbonyl]-4-hydroxy-6-methyl-2（1H）-pyridinones

1 INTRODUCTION Recently, compounds containing pyrazole, imida- zole, triazole (including benzotriazole), pyridine, tetrazole and indole have attracted much interest because of their fungicidal activity, plant-growth regulating activity and antibacterial activity[1～3]. Schiff bases also constitute a good type of biolo- gically active substructures[4～7]. Studies of pyri- dine Schiff base-type fungicides have been repor- ted[8]. However, some structures of pyridine com- pounds containing h…     

Microwave activated synthesis of 2-aryl-quinazolin-4（3H）ones

A highly efficient synthesis of 2-aryl-quinazolin-4(3H)ones was performed by one-pot oxidative heterocyclization of 2- aminobenzamide with aldehydes in the presence of potassium permanganate in dimethylacetamide under microwave irradiation.     

Crystal Structure and Biological Activities of （R）-N′-[2-（4-Methoxy-6-chloro）-pyrimidinyl]- N-[3-methyl-2-（4-chlorophenyl）butyryl]-urea

1 INTRODUCTION The acyl ureas are a kind of high biological acti- vity compounds with low toxicity to mammals, birds, fish, amphibians, etc., and significant organic synthe- sis intermediates working extensively as insecticides, pesticides, fungicides and herbicides in agrochemi- cal industry[1～7]. While pyrimidinyl derivatives show excellent biological activities in the development of pesticide, and are used to develop high effective and high select herbicides. For example, pyrimidiny su…     

A Rapid Parallel Synthesis of 2-Dialkylamino-4（3H）-quinazolinones

2-Dialkylamino-4(3H)-quinazolinones 4 were rapidly synthesized by a solution-phase parallel synthetic method, which includes aza-Wittig reaction of iminophosphorane 1 with aromatic isocynate to give carbodiimide 2 and subsequent reaction of 2 with various aliphatic secondary amine in a parallel fashion.     

2-氨基-6-氟-9-(4-羟基-3-羟甲基丁基)嘌呤的合成

报道了2-氨基-6-氟-9-(4-羟基-3-羟甲基丁基)嘌呤(1)的合成, 通过对起始原料2-氨基-6-氯-9-(4-乙酰氧基-3-乙酰氧甲基丁基)嘌呤(2)水解脱去乙酰基, 得到2-氨基-6-氯-9-(4-羟基-3-羟甲基丁基)嘌呤(3). 化合物3与三甲胺乙醇溶液在混合溶剂[V(THF)∶V(DMF)＝3∶1]中反应得到相应的氯化铵盐4, 然后与KF在DMF溶剂中反应, 得到化合物1. 产品经UV-vis, IR, ¹H NMR, ¹⁹F NMR和MS表征. 考察了反应温度、氟化试剂等因素对氟化反应的影响, 为6位含氟的嘌呤核苷类化合物的合成提供了一种直接、简易的新方法.     

A Convenient Synthesis of 6,8-Dimethoxy-3-[（2-（4-methoxyphenyl）ethyl）isocoumarin

6,8-Dimethoxy-3-[2-（4-methoxyphenyl）ethyl]isocoumarin was synthesized by condensation of 5,7-dimethoxyhompophthalic acid with 3-（4-methoxyphenyl）propanoyl chloride. The structure of the synthesized compound was confirmed by its mass spectrometric studies. The synthesized compound serves as a model for synthesis of DL-agrimonolide.     

Synthesis and Crystal Structure of 2-Amino-4- chloro-5-（4-methylbenzyl）-6-methylpyrimidine

The title compound 2-amino-4-chloro-5-(4-methylbenzyl)-6-methylpyrimidine (C26H28Cl2N6, Mr = 495.44) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 14.892(7), b = 6.129(3), c = 14.889(7) , β = 109.795(8)°, V = 1278.7(10) 3, Z = 2, F(000) = 520, Dc = 1.287 g/cm3, μ = 0.280 mm-1, the final R = 0.0577 and wR = 0.1589 for 1357 observed reflections with I > 2σ(I). A total of 6091 reflections were collected, of which 2257 were independent (Rint = 0.033). The X-ray analysis reveals that the chlorine atom and methyl of the title compound are disordered.     

2-羟基-4-磺酰氨基苯重氮氨基偶氮苯的合成及与镉的显色反应

合成了 2 羟基 4 磺酰氨基苯重氮氨基偶氮苯 (HSDAA) ,并研究了在TritonX 1 0 0表面活性剂存在下HSDAA与镉的显色反应。在pH 8 5～ 1 0 5的Na2 B4 O7 NaOH缓冲溶液中 ,该试剂与镉生成 2∶1型深红色配合物。配合物的最大吸收峰位于 5 2 5nm处 ,表观摩尔吸光系数达 1 84× 1 0 5L·mol- 1·cm- 1。ρ(Cd2 + )在 0～ 480 μg/L范围内符合比耳定律。用拟定方法测定样品中的微量镉 ,结果满意。     

反-4-(反-4'-正丙基环已基)环已醇的合成与表征

环己烷类液晶因具有高度的稳定性,较宽的相列相温区而受到人们的青睐。反-4-(反-4’-正丙基环己基)环己醇(trans-3HHE)是一种合成环己烷类液晶的重要中间体,它可通过酶选择性催化和顺式构型异构化二种方法合成。文献报道顺式构型异构化法是：4-(反-4’-正丙基环己基)苯酚以铑／碳或铑／氧化铝为催化剂,在酸性介质条件下进行加氢反应,     

The new convenient synthesis of fluorinated Penciclovir analogues 9-(4-fluoro-3-hydroxymethylbutyl) guanine (FHBG) and 2-amino-6-fluoro-9-(4-hydroxy-3-hydroxymethylbutyl) purine (6-Fluoropenciclovir)

9-(4-Hydroxy-3-hydroxymethylbutyl) guanine (Penciclovir) is a potent and selective inhibitor of members of the herpes virus family. A new convenient synthesis of fluorinated Penciclovir analogues 9-(4-fluoro-3-hydroxymethylbutyl) guanine (FHBG) and 2-amino-6-fluoro-9-(4-hydroxy-3-hydroxy-methylbutyl) purine (6-Fluoropenciclovir) were described. The structures of the products were characterized by UV, IR, ¹H NMR, ¹⁹F NMR spectra and MS.     

Stereocontrolled synthesis of (-)-kainic acid from trans-4-hydroxy-L-proline

[reaction: see text] A highly stereoselective synthesis of (-)-kainic acid has been achieved in 14 steps and >7% overall yield starting from inexpensive trans-4-hydroxy-L-proline. The key steps are diastereoselective enolate alkylation and cuprate substitution reactions.     

Synthesis and herbicidal activity of 2-cyano-3-(2-fluoro-5-pyridyl)methylaminoacrylates

A series of 2-cyano-3-(2-fluoro-5-pyridyl)methylaminoacrylates were synthesized as herbicidal inhibitors of photosystem II (PSII) electron transport. 2-Fluoro-5-pyridinemethylamine was prepared from 2-amino-5-methylpyridine, subsequent reaction with 2-cyano-3,3-dimethylthioacrylates or 2-cyano-3-methoxyacrylates to yield these title compounds. All of these compounds were confirmed by ¹H NMR, IR, mass spectrum and elemental analyses. Their herbicidal activities were evaluated. All of the title compounds showed excellent herbicidal activities to amaranth pigweed and rape in post-emergence treatment. At the rate of 150 g/ha, one compound exhibited similar activity to Cl-analogue. The replacement of chlorine by fluorine group showed the same herbicidal activity.     

A re-investigation of the Fries rearrangement of 3-chlorophenyl acetate and synthesis of 2-azido-1-(4-(benzyloxy)-2-chlorophenyl)ethanone from 4-bromo-3-chlorophenol

The Fries rearrangement of 3-chlorophenyl acetate provided the expected 4-chloro-2-hydroxy-acetophenone as the major product and 2,4-diacetyl resorcinol and 2-chloro-4-hydroxy-acetophenone as minor products. 4-Benzyloxy-2-chloroacetophenone was prepared by a Heck reaction and then elaborated to 4-benzyloxy-2-chlorophenacyl azide.     

New Facile Synthesis of 2-Aryloxy-5-(2-furfurylidene)- 4H-imidazolin-4-ones

Many N-heterocycles including 4H-imidazolin-4-ones exhibit biological activities1-3. Some derivatives of 5-(2-furfurylidene)-4H-imidazolin-4-one were found to show good antiinflammatory activity4. They can be synthesized by condensation of furfural with 5- unsubsituted 4H-imidazolin-4-ones or from corresponding oxazolones5,6. However, no synthesis of 2-aryloxy substituted 5-(2-furfurylidene)-4H-imidazolin-4-one was reported. Recently, aza-Wittig reaction has received increased attention …     

Microwave promoted one-pot synthesis of 3-(2''-amino-3''-cyano-4''-arylpyrid-6''-yl) coumarins

A facile procedure for the synthesis of 3-(2'-amino-3'-cyano-4'-arylpyrid-6'-yl) coumarins are being reported starting from 3-acetylcoumarin, aromatic aldehydes and malononitrile. The reactions were carded out on microwave irradiation in good yield with short time and easy work-up. The structures of all the compounds have been confirmed on the basis of their analytical, IR,1H NMR,and mass spectral data.     

Synthesis of 2-(4-Hydroxy-6-methyl-2-oxo-2H-pyran-3-carbonyl)-6,6-dimethyl-3-phenyl-3,5,6,7-tetrahydro-2H-benzofuran-4-one Derivatives via Multicomponent Reaction

A sequential one-pot, two-step reaction for an efficient preparation of 2-(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-carbonyl)-6,6-dimethyl-3-phenyl-3,5,6,7-tetrahydro-2H-benzofuran-4-one derivatives has been described. One-pot reaction of in situ–formed benzopyran-substituted pyridinium ylides with aromatic aldehydes and dimedone gives corresponding 2,3-dihydrofurans in good yields. The structures of all the newly synthesized compounds were confirmed from their analytical and spectral data.     

6-Endo Heck Cyclization of 3-(2-Iodophenoxy)methylbenzofurans: A Useful Approach to Pterocarpenes

Mitsunobu coupling of 3-hydroxymethylbenzofurans with o-iodophenols affords 3-(2-iodophenoxy)methylbenzofurans which under go a useful 6-endo Heck cyclization under Jeffery conditions to afford pterocarpene-type heterocycles. The unsubstituted parent pterocarpene thus prepared was readily converted to coumestan via subsequent PCC oxidation.

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