scholarly journals SYNTHESIS AND CONFORMATIONS OF p-(ACETAMIDO)-BUTOXYCALIX[4]ARENE AND p-(BENZAMIDO)-BUTOXYCALIX[4]ARENE

2010 ◽  
Vol 7 (2) ◽  
pp. 166-171
Author(s):  
Firdaus Firdaus ◽  
Jumina Jumina ◽  
Hardjono Sastrohamidjojo
Keyword(s):  
1H Nmr ◽  
Benzoyl Chloride ◽  
Room Temperature ◽  
Acetyl Chloride ◽  
13C Nmr Spectroscopy ◽  
Inert Atmosphere ◽  
Cone Conformation ◽  
Partial Cone ◽  
Temperature Method ◽  
Spectral Patterns

The conversion of p-(amino)butoxycalix[4]arene, 1, to p-(acetamido)butoxy-calix[4]arene, 2, and p-(benzamido)butoxycalix[4]arene, 3, via acetylation and benzoylation reactions, respectively have been conducted. The acetylation reactions was conducted by reflux method and room temperature method. The reflux method was conducted by refluxed a solution of 1 and acetic anhydride in acetic acid glacial solvent for 12 hours to result 2 in 53.8% yield; while the room temperature method was conducted by stirred a solution of 1, acetyl chloride, and dry pyridine in dry toluene solvent and inert atmosphere at room temperature for 24 hours to result 2 in 97.8% yield. By the room temperature method and using benzoyl chloride, the compound 3 was obtained in 67.1% yield. Structures of the both compounds were confirmed using IR, 1H NMR, and 13C NMR spectroscopy methods. Pursuant to the 1H-NMR spectral patterns of their bridge methylene and calix aryl protons, they were known that the compound 3 exist in partial cone conformation; whereas the compound 2 exist in partial cone, cone, and 1,2-alternate conformations where the partial cone was the main conformer.   Keywords: p-(amino)butoxycalix[4]arene, p-(acetamido)butoxycalix[4]arene, p-(benzamido)butoxycalix[4]arene,

Metal Ion Binding to Calixarenes: Pendent Arm Coordination Assisted by Self-Inclusion

1994 ◽  
Vol 47 (6) ◽  
pp. 1185 ◽  
Author(s):  
JM Harrowfield ◽  
M Mocerino ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Structural Characterization ◽  
Metal Ion ◽  
Room Temperature ◽  
Ion Binding ◽  
Metal Ion Binding ◽  
Cone Conformation ◽  
X Ray ◽  
Partial Cone ◽  
Arm Coordination

The synthesis and room-temperature single-crystal X-ray structural characterization of 25,27- di(allyloxy)-5,17-di-t-butyl-26,28-dimethoxycalix[4]arene are recorded. Crystals are monoclinic, C2/c, a 29.089(5), b 10.742(2), c 26.218(8) Ǻ, β 110.09(2)°, Z = 8; the structure was refined to a residual of 0.065 for 4103 independent 'observed' [I > 3σ(I)] reflections. The flattened partial cone conformation of the molecule allows inclusion of one of the methoxy substituents in a way which could block inclusion of a metal ion capable of polyhapto aromatic coordination and which may therefore explain why solution n.m.r. measurements indicate that silver(I) binds to the pendent alkene groups.

scholarly journals Reactions of MoCl5 and MoO2Cl2 with 4-Phenylimidazole-2-Thiol and 2-Thiazoline-2-Thiol

2020 ◽  
Vol 36 (6) ◽  
pp. 1096-1102
Author(s):  
Deepika Rani ◽  
Gursharan Singh ◽  
Seema Sharma
Keyword(s):  
Liquid Nitrogen ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Room Temperature ◽  
Inert Atmosphere ◽  
Molar Ratios ◽  
Vacuum Line

Reactions of MoCl5/MoO2Cl2 with 4-phenylimidazole-2-thiol/2-thiazoline-2-thiol in CH3CNsolvent in 1:1/1:2 molar ratios have been carried out at room temperature. Products obtained MoCl3(C9H7N2S)(CH3CN), [1];MoCl2(C9H7N2S)(CH3CN), [2]; Mo2OCl4(C9H8N2S)2, [3] and Mo4O2Cl12(C9H7N2S)4, [4]; MoO2Cl3(C3H5NS2)2, [5] and Mo2O4Cl3(C3H5NS2)2, [6] have been analyzed and characterizedby elemental analysis, FTIR, 1H NMR and LC-MS techniques. Compounds being moisture and air sensitive, these have been prepared in inert atmosphere using vacuum line and liquid nitrogen cooled traps. Fragments obtained in LC-MS spectra support the formulae derived.

scholarly journals Reactions of MoCl5 and MoO2Cl2 with 4-Phenylimidazole-2-thiol and 2-Thiazoline-2-thiol

2020 ◽  
Vol 36 (6) ◽  
pp. 1096-1102
Author(s):  
Deepika Rani
Keyword(s):  
Liquid Nitrogen ◽  
1H Nmr ◽  
Elemental Analysis ◽  
Room Temperature ◽  
Inert Atmosphere ◽  
Molar Ratios ◽  
Vacuum Line

Reactions of MoCl5/MoO2Cl2 with 4-phenylimidazole-2-thiol/2-thiazoline-2-thiol in CH3CN solvent in 1:1/1:2 molar ratios have been carried out at room temperature. Products obtained MoCl3(C9H7N2S)(CH3CN),[1]; MoCl2(C9H7N2S)(CH3CN), [2]; Mo2OCl4(C9H8N2S)2, [3] and Mo4O2Cl12(C9H7N2S)4, [4]; MoO2Cl3(C3H5NS2)2, [5] and Mo2O4Cl3(C3H5NS2)2, [6] have been analyzed and characterized by elemental analysis, FTIR, 1H NMR and LC-MS techniques. Compounds being moisture and air sensitive, these have been prepared in inert atmosphere using vacuum line and liquid nitrogen cooled traps. Fragments obtained in LC-MS spectra support the formulae derived.

scholarly journals SYNTHESIS OF THIOMETHYLATED CALIX[4]RESORCINARENE BASED ON FENNEL OIL VIA CHLOROMETHYLATION

2011 ◽  
Vol 11 (1) ◽  
pp. 1-8 ◽  
Author(s):  
Suryadi Budi Utomo ◽  
Jumina Jumina ◽  
Dwi Siswanta ◽  
Mustofa Mustofa ◽  
Naresh Kumar
Keyword(s):  
Melting Point ◽  
Sodium Hydroxide ◽  
1H Nmr ◽  
Sodium Hydroxide Solution ◽  
Starting Material ◽  
Cone Conformation ◽  
Hydroxide Solution ◽  
Partial Cone ◽  
Ft Ir ◽  
Fennel Oil

A research has been conducted to synthesize thiomethylated-C-4-methoxyphenylcalix[4]resorcinarene using fennel oil as a starting material. The synthesis was carried out in four steps i.e. (1) oxidation of anethole to yield p-anisaldehyde, (2) HCl-catalyzed condensation of p-anisaldehyde with resorcinol, (3) chloromethylation of C-4-methoxyphenylcalix[4]resorcinarene with paraformaldehyde and HCl in the presence of ZnCl2 to yield tetrakis-chloromethyl-C-4-methoxyphenylcalix[4]resorcinarene, and (4) reaction of tetrakis-chloromethyl-C-4-methoxyphenylcalix[4]resorcinarene with thiourea followed by hydrolysis with sodium hydroxide solution to yield tetrakis-thiomethyl-C-4-methoxyphenylcalix[4]resorcinarene. The prepared compounds were characterized based on melting point, FT-IR, and NMR spectrometers. According to the analysis of 1H-NMR spectrometer, C-4-methoxyphenylcalix[4]resorcinarene and tetrakis-chloromethyl-C-4-methoxyphenylcalix[4]resorcinarene were observed in the chair or flattened partial cone conformation, while tetrakis-thiomethyl-C-4-methoxyphenylcalix[4]resorcinarene tend to exist in the crown or cone conformation.

Friedel-Crafts acylation of antiaromatic norcorrole: electronic and steric modulation of the paratropic current

2021 ◽  
Author(s):  
Sha Li ◽  
Oskar Smaga ◽  
Yahan Sun ◽  
Xiaofang Li ◽  
Miłosz Pawlicki ◽  
...  
Keyword(s):  
Room Temperature ◽  
Acetyl Chloride ◽  
Acyl Chlorides

Acyl chlorides react with norcorrolatonickle(II) in dichloromethane in the presence of AlCl3 at room temperature affording two isomeric monoketone derivatives in moderate yields. For acetyl chloride, also diketones were detected...

scholarly journals SYNTHESIS, CHARACTERIZATION AND ANTIOXIDANT ACTIVITY OF 7-HYDROXY-3',4'-DIMETHOXYFLAVONE

2012 ◽  
Vol 12 (2) ◽  
pp. 146-151 ◽  
Author(s):  
Elfi Susanti VH ◽  
Sabirin Matsjeh ◽  
Tutik Dwi Wahyuningsih ◽  
Mustofa Mustofa ◽  
Tri Redjeki
Keyword(s):  
Aqueous Solution ◽  
Antioxidant Activity ◽  
Sodium Hydroxide ◽  
Spectral Data ◽  
1H Nmr ◽  
13C Nmr ◽  
Room Temperature ◽  
Antioxidant Activities ◽  
Oxidative Cyclization ◽  
Dpph Method

Synthesis of flavones and their derivatives has attracted considerable attention due to their significant pharmaceutical effects. 7-hydroxy-3',4'-dimethoxyflavone has been synthesized and its antioxidant activity has been investigated. Flavone was synthesized by oxidative cyclization of chalcone. 2',4'-dihydroxy-3,4-dimethoxychalcone was prepared by Claisen-Schmidt condensation of 2,4-dihydroxyacetophenones with 3,4-dimethoxybenzaldehydes in the presence of aqueous solution of sodium hydroxide and ethanol at room temperature. Oxidative cyclization of 2',4'-dihydroxy-3,4-dimethoxychalcone was done by using I2 catalyst in DMSO to form 7-hydroxy-3',4'-dimethoxyflavone. The synthesized compounds were characterized by means of their UV-Vis, IR, 1H-NMR and 13C-NMR spectral data. The compound was tested for their antioxidant activities by DPPH method.

A novel room temperature method to nanocrystalline Ag2Se

1999 ◽  
Vol 34 (6) ◽  
pp. 877-882 ◽  
Author(s):  
Wenzhong Wang ◽  
Yan Geng ◽  
Yitai Qian ◽  
Mingrong Ji ◽  
Yi Xie
Keyword(s):  
Room Temperature ◽  
Temperature Method
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