1927-68-0Relevant articles and documents
Crystal structure, thermal decomposition mechanism and catalytic performance of hexaaquaaluminum methanesulfonate
Wang, Rui,Li, Rongrong,Jiang, Heng,Gong, Hong,Bi, Yanfeng
, p. 1327 - 1338 (2017/04/06)
Hexaaquaaluminum methanesulfonate crystals, [Al(H2O)6][CH3SO3]3 were synthesized by a hydrothermal reaction of Al(OH)3 with methanesulfonic acid. Single-crystal diffraction determination revealed that Al3+ was coordinated by six water molecules in octahedral geometry, while the CH3SO3 – anion connected with Al3+ through coordinated water molecules by hydrogen bonds. The six-coordinate environment of Al was also determined by 27Al MAS NMR measurement. Thermogravimetric analysis and Fourier transform infrared spectroscopy showed that the decomposition intermediate at 265–365?°C was Al2(μ-OH)(CH3SO3)5 and the final product was amorphous Al2O3 residue with about 0.8 wt% SO3 at 520–800?°C. A pure phase of [Al(H2O)6][CH3SO3]3 was confirmed by powder X-ray diffraction analysis. Esterification of n-butyric acid with n-butanol and ketalization of cyclohexanone with glycol catalyzed by [Al(H2O)6][CH3SO3]3 and Al2(μ-OH)(CH3SO3)5, respectively, proceeded in 100% yield by continuously removing the produced water. In the case of tetrahydropyranylation of n-butanol at room temperature in dichloromethane, the catalytic activity of [Al(H2O)6][CH3SO3]3 was much lower than that of Al2(μ-OH)(CH3SO3)5. Furthermore, both [Al(H2O)6][CH3SO3]3 precursor and Al2(μ-OH)(CH3SO3)5 catalysts could be recycled.
3,5-Dinitrobenzoic acid catalyzed synthesis of 2,3-unsaturated O- and S-glycosides and tetrahydropyranylation of alcohols and phenols
Bodipati, Naganjaneyulu,Palla, Srinivasa Rao,Komera, Venkateshwarlu,Peddinti, Rama Krishna
supporting information, p. 6878 - 6881 (2015/02/02)
A simple procedure for the synthesis of 2,3-unsaturated glycosides in acetonitrile and tetrahydropyranylation of alcohols and phenols in dichloromethane in the presence of 3,5-dinitrobenzoic acid is described. A variety of alcohols and thiols are reacted with glycals to give the desired products in high yields with high α-selectivity.
Solvent-free tetrahydropyranylation of alcohols catalyzed by amine methanesulfonates
Wang, Rui,Sun, Mingzhu,Jiang, Heng
experimental part, p. 61 - 67 (2012/02/16)
A comparative study of tetrahydropyranylation of alcohols under various solvents or solvent-free conditions using different amine methanesulfonates as catalysts shows that tetrahydropyranyl ethers of alcohols are obtained under solvent-free conditions in good yields using catalytic amounts of triethylenediamine methanesulfonate, 1,6-hexanediamine methanesulfonate, diethylenetriamine methanesulfonate and pyridine methanesulfonate, respectively. The reaction occurs readily in short times at room temperature catalyzed by these catalysts, especially triethylenediamine methanesulfonate. Some of the major advantages of this procedure are that the catalysts are environmentally friendly, highly effective, and easy to prepare and handle. The reaction is also clean and needs no solvent, and the work-up is very simple.