1—[2—（N—甲基—N—取代苄基）氨基—2—（4—叔丁基苯基）乙？…

根据氮唑类和苄胺类抗真菌药物的构效关系和作用机理,设计合成了２３种１－「２－（Ｎ－甲基－Ｎ－取代苄基）氨基－２－（４－叔丁基苯基）乙基」－１Ｈ－１,２,４－三唑类化合物,其结构经元素分析、红外光谱及核磁共振谱分析 证实。体外抑菌实验结果表明：目标化合物对常见的９种致病真菌均有一定活性,对浅表真菌活性优于深部真菌,其中化合物３,４,６,１０,１２,１４和１５对羊毛样小孢菌具有较强的活性。     

1-[2-(N-甲基-N-取代苄基)氨基-2-(4-叔丁基苯基)乙基]-1H-1,2,4-三唑类化合物的合成及抗真菌活性

根据氮唑类和苄胺类抗真菌药物的构效关系和作用机理,设计合成了23种1-[2-(N-甲基-N-取代苄基)氨基-2-(4-叔丁基苯基)乙基]-1H-1,2,4-三唑类化合物,其结构经元素分析、红外光谱及核磁共振谱分析证实.体外抑菌实验结果表明:目标化合物对常见的9种致病真菌均有一定活性,对浅表真菌活性优于深部真菌,其中化合物3,4,6,10,12,14和15对羊毛样小孢子菌具有较强的活性.     

Synthesis of (Z)-4-hydroxytamoxifen and (Z)-2-[4-[1-(p-hydroxyphenyl)-2-phenyl]-1butenyl]phenoxyacetic acid

The synthesis of (Z)-4-hydroxytamoxifen and (Z)-2-[4-[1-(p-hydroxyphenyl)-2-phenyl]-1-butenyl]phenoxyacetic acid was accomplished using a McMurry reaction as the key step. The perfluorotolyl derivatives of the McMurry products enabled the separation of the minor undesirable geometrical isomer. The methodology proceeds without E,Z isomerization, employs a very mild final debenzylation step compatible with a large array of functional groups, and can be applied to the generation of a variety of 4-hydroxytamoxifen analogues.     

配合物[1-(4′-bromo-2′-fluorobenzyl)pyridinium]2[Ni(mnt)2]和[1-(4′-bromo-2′-fluorobenzyl)pyrazinium]2[Ni(mnt)2](mnt2-=maleonitriledithiolate dianion)的合成及晶体结构

本文报道两个含双(马来二氰基二硫烯)镍(Ⅱ)配合物阴离子的离子对化合物。对阳离子为1-(4′-溴-2′-氟苄基)吡啶 盐时,生成配合物1。晶体数据:三斜晶系,空间P1群,a=0.7086(2)nm,b=1.0968(3)nm,c=1.1775(3)nm,α=69.914(5)°,β=89.495(5)°,γ=74.765(5)°,V=0.8259(4)nm³,Z=1。对阳离子为1-(4′-溴-2′-氟苄基)吡嗪鎓盐时,生成配合物2。晶体数据:单斜晶系,空间群P2₁/n,a=0.71554(17)nm,b=1.4262(3)nm,c=1.6725(4)nm,β=100.396(4)°,V=1.6788(7)nm³,Z=4。两个配合物中,阴离子为拟平面结构,镍原子均位于对称中心。变换对阳离子上的芳环种类对晶体的堆积结构产生影响。     

Synthesis and antiestrogenic activity of the compounds related to the metabolites of (E)-4-[1-[4-[2-(dimethylamino)ethoxy]phenyl]- 2-(4-isopropylphenyl)-1-butenyl]phenyl monophosphate (TAT-59) [corrected

The metabolites of (E) [corrected]-4-[1-[4-[2-dimethylamino)ethoxy]phenyl]- 2-(4-isopropylphenyl)-1-butenyl]phenyl monophosphate, TAT-59, (1), a potent antitumor agent for hormone-dependent tumors, and derivatives of TAT-59 were synthesized to confirm its proposed structure. The structure and the Z-configuration of the metabolites (2a-8a) were confirmed by comparison with synthesized authentic compounds. All of the metabolites and the derivatives of TAT-59 were tested for a binding affinity toward estrogenic receptors in vitro and antiuterotrophic activity in vivo. Most of the metabolites possessed remarkable binding affinity toward estrogenic receptors as well as fairly good antiuterotrophic activity.     

CRYSTAL STRUCTURE OF THE METHYL 4—（N—（1—OXYPROPYL）—N—PHENYLAMINO]—1—[2—（2—THIENYL）ETHYL]—4—PIPERIDINECARBOXYLATE（R31826）HYDROCHLORIDE

<正> C22H28N2O3S.HCl, Mr = 436.9, triclinic,P1;a=8.557(3),b= 10.299(2),c= 13.894(2)A;α= 99.25(1),β=86.64(2),γ= 107.68(2)°;V= 1151.2(3)A3,Z= 2, DC = 1.27g/cm3,R=0.064. The torsion angle C(14)-C(1)-N(2)-0(19) in the title compound is 137.5 being much larger than that (106°) in R30730. The dihedral angle between mean planes of the thiophene ring and piperidine ring is about 83 .     

Ambidentate Properties of Asymmetric Substituted Imidazoles. Direction of Benzylation of 2-[N-(4-Chlorophenyl)carbamoyl]methylthio-4-phenyl-1H-imidazole

On the basis of ¹H-¹H two dimensional NMR spectroscopy (NOESY) it has been unambiguously shown that the benzylation of 2-[N-(4-chlorophenyl)carbamoyl]methylthio-4-phenyl-1H-imidazole occurs at the N₍₁₎ atom. This data was confirmed by comparison of the properties of the alkylation product obtained with the corresponding N₍₃₎-benzylimidazole isomer synthesized independently. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 882–886, June, 2005.     

1-[2-（2-Methoxyphenylthio） benzyl]-4-arylpiperazines derivatives： Synthesis and evaluation for dual 5-HT1A/SSRI activities

A series of 1-[2-（2-methoxyphenylthio） benzyl]-4-arylpiperazines derivatives was designed and synthesized based on 5-HT1A/ SSRI drugs design strategies. The synthesized compounds were evaluated for their dual 5-HT1A/5-HTT activities. 2007 Ai Jun Li. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.     

The preparation of 8-[4-[4-(2-pyrimidinyl)-1-piperaziny]butyl]-8-azaspiro[4,5] decane-7,9-dione hydrochloride

8-[4-[4-(2-Pyrimidinyl)-1-piperaziny]butyl]-8-azaspiro [4,5] decane-7,9-dione hydrochloride (buspirone hydrochloride) was obtained in one pot with a 51.8% overall yield. The key intermediate, 1-(2-pyrimidinyl) piperazine, was synthesized through chlorination and cyclization condensation reaction with diethanolamine as initial material. This modified protocol has the notable advantages of mild reaction condition, convenient operation, and high overall yield.     

Synthesis of 3,5-diaryl-4-(1H-imidazol- 2-yl)-1H-pyrazoles from 2-phenacyl- 1H-imidazole

A method of synthesis is proposed for previously unknown 3,5-diaryl-4-(1H-imidazol-2-yl)-1H-pyra-zoles based on the thermal intramolecular cyclocondensation of aroylhydrazones of 2-phenacyl-1H-imidazole.     

Synthesis and Crystal Structure of 2-（4-Chlorophenyl）-1,4,5-triphenyl-1H-imidazole

The compound 2-(4-chlorophenyl)-1,4,5-triphenyl-1H-imidazole(1,C27H19ClN2) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal of 1 belongs to the triclinic system,space group P with a = 10.3350(19),b = 10.238(2),c = 11.201(2) ,α = 85.957(16),β = 83.148(15),γ = 66.467(15)°,V = 1078.5(4) 3,Mr = 406.89,Z = 2,F(000) = 422,Dc = 1.257 g/cm3,μ = 0.193 mm-1,T = 298(2) K,S = 1.092,R = 0.0702 and wR = 0.1258.The imidazole ring system is planar and makes a dihedral angle of 40.3° with the chlorobenzene ring.     

Novel Synthesis of 1-(1,2,3,5,6,7-Hexahydro- s-indacen-4-yl)-3-[4-(1-hydroxy-1-methyl-ethyl)-furan-2-sulfonyl]urea,an Anti-inflammatory Agent

Abstract

A novel synthesis of the anti-inflammatory agent 1-(1,2,3,5,6,7- hexahydro-s-indacen-4-yl)-3-[4-(1-hydroxy-1-methyl-ethyl)-furan-2-sulfonyl] urea 1 is described. Sulfonamide 5 was prepared starting from ethyl 3-furoate 2. Key steps were a one-pot sulfonylation with chlorosulfonic acid in methylene chloride followed by pyridinium salt formation and reaction with phosphorus pentachloride to provide ethyl 2-(chlorosulfonyl)-4-furoate 7. This sulfonyl chloride was treated with ammonium bicarbonate to form sulfonamide 8, followed by treatment with excess methyl magnesium chloride to provide 4-(1-hydroxy-1-methyl-ethyl)-furan-2-sulfonamide 5. 4-Isocyanato-1,2,3,5,6,7-hexahydro-s-indacene 16 was prepared from indan in five steps. The formation of the desired sulfonyl urea was carried out both with the isolated isocyanate 16 and via an in situ method.