Preparation, characterization and use of 1,3-disulfonic acid imidazolium hydrogen sulfate as an efficient, halogen-free and reusable ionic liquid catalyst for the trimethylsilyl protection of hydroxyl groups and deprotection of the obtained trimethylsilanes
摘要:
Novel 1,3-disulfonic acid imidazolium hydrogen sulfate, a halogen-free ionic liquid, is a recyclable and eco-benign catalyst for the trimethylsilyl protection of hydroxyl groups at room temperature under solvent free conditions to afford trimethylsilanes in excellent yields (92-100%) and in very short reaction times (1-5 min). Deprotection of the resulting trimethylsilanes can also be achieved using the same catalyst in methanol. The catalyst was characterized by IR. H-1 NMR, C-13 NMR and MS studies. All the products were extensively characterized by IR, H-1 NMR, MS, and elemental and melting point analyses. This new method consistently has the advantages of excellent yields and short reaction times. Further, the catalyst can be recovered and reused for several times without loss of activity. The work-up of the reaction consists of a simple separation, followed by concentration of the crude product and purification. (C) 2012 Elsevier B.V. All rights reserved.
A Highly Efficient Method for the Silylation of Alcohols, Phenols, and Naphthols Using HMDS in the Presence of Zinc Oxide (ZnO) as Economical Heterogeneous Catalyst
作者:Hamid Reza Shaterian、Majid Ghashang
DOI:10.1080/10426500701569406
日期:2007.12.24
Variety alcohols, phenols, and naphthols were effectively converted into their corresponding trimethylsilyl ether with hexamethyldisilazane in the presence of zinc oxide under very mild and ambient conditions with short reaction time in good to excellent yields.
Alumina sulfuricacid as a recyclable catalyst conducts the transformation of various types of alcohol, phenols, and oximes with hexamethyldisilazane (HMDS) to the corresponding O-trimethylsilylated compounds in good to excellent yields under mild and ambient conditions with short reaction times. The method is highly selective for the conversion of primary alcohols in the presence of secondary and
An efficient method for the silylation of hydroxyl groups with hexamethyldisilazane (HMDS) catalyzed by aluminum tris(dihydrogen phosphate) under solvent-free and ambient conditions
A highly efficient and mild procedure for the trimethylsilylation of a wide variety of alcohols, including primary, benzylic, secondary, hindered secondary, tertiary, phenols, and oximes with hexamethyldisilazane (HMDS), using Al(H2PO4)3 as a recyclable heterogeneous catalyst at room temperature in a few minutes with excellent yields under solvent-free conditions is described.Key words: trimethylsilylation
Alumina Perchloric Acid (Al<sub><b><i>2</i></b></sub>O<sub><b><i>3</i></b></sub>-HClO<sub><b><i>4</i></b></sub>) as an Efficient Heterogeneous Catalyst for Modified Preparation of Trimethylsilyl Ethers
for the trimethylsilylation of a wide variety of alcohols, including primary, benzylic, secondary, hindered secondary, tertiary, phenols, and oximes with hexamethyldisilazane (HMDS) using alumina perchloric acid (Al 2 O 3 -HClO 4 ) as recyclable heterogeneous catalyst in excellent yields with short reaction times (3−65 min) under ambient conditions is described.
Multicyclic Poly(ether ketone)s Obtained by Polycondensation of 2,6,4‘-Trifluorobenzophenone with Various Diphenols
作者:Hans R. Kricheldorf、Radka Hobzova、Lali Vakhtangishvili、Gert Schwarz
DOI:10.1021/ma050037+
日期:2005.5.1
2,6,4‘-Trifluorobenzophenone (TFB) was polycondensed with silylated 4,4‘-dihydroxybiphenyl (DHBP) or silylated bisphenol A in N-methylpyrrolidone by means of K2CO3 as catalyst and HF acceptor. At constant concentration (0.08 mol/L) the feed ratio was varied from 1.0/1.0 to 1.0/1.5. For polycondensations of DHBP cross-linking was observed for feed ratios above 1.0/1.1, whereas no gelation occurred with