Inorganic oxides reaction procedure

Alumina supported sodium metaperiodate, which can be prepared by soaking the inorganic support with a hot solution of sodium metaperiodate, was also found to be a very convenient reagent for the selective and clean oxidation of sulphides to sulphoxides79. The oxidation reaction may be simply carried out by vigorous stirring of this solid oxidant with the sulphide solution at room temperature. As may be expected for such a procedure, solvent plays an important role in this oxidation and ethanol (95%) was found to be... 

Reactions carried out on the surface of inorganic oxides allow convenient high-yield and selective syntheses of various metal carbonyl complexes and clusters, starting from easily available materials (Tables 16.1-16.3). The synthetic procedures are straightforward and the recovery of products is easy. Since the use of a solid as reaction medium is not Umited in the manner in solution by boiling points and by the thermal instabiUty of some solvents, it is possible to work at atmospheric pressure even at rather high temperatures. Therefore, in many cases, yields and pressure are better and lower, respectively, than those of the traditional syntheses in solution (Tables 16.4—16.6). 

In the early eighties, a new method for the deposition of transition metal ion monolayer on the surfaces of inorganic oxides was developed in our laboratory [3]. The essential step of this method is the selective reaction of the surface hydroxyl groups with transition metal alkoxide molecules [3,4]. The adopted procedure allows the design of catalysts containing a strictly determined number of transition metal monolayers or sandwich-type catalysts with different metals monolayers anchored to the surface of the carrier. 

The use of the surface of inorganic oxides as reaction media enables selective and high-yield syntheses of a variety of neutral and anionic osmium carbonyl clusters starting from simple and readily available materials. The procedures are simple and straightforward. Because the use of a solid as a reaction medium is not limited, as in solution, by boiling points, it is possible to work at atmospheric pressure even at relatively high temperatures. 

Preparation of Aroyl Chlorides. Substituted benzylidene chlorides (trichloromethylarenes) can be converted to the corresponding substituted benzoyl chlorides (aroyl chlorides) with hexamethyldisiloxane in the presence of a catalytic amount of iron(III) chloride (eq 4). These mild reaction conditions offer a distinct advantage over procedures which err5>loy inorganic oxides and high temperatures to achieve the transformation. ... 

Method E - catalytic procedure (typical procedure). Benzaldehyde (106 mg, 1.0 mmol), methyl bromoacetate (165 mg, 1.1 mmol), triphenyl phosphite (356 mg, 1.2 mmol), dibutyl telluride (48 mg, 0,2 mmol), KjCOj (179 mg, 1.3 mmol) and THF (4 mL) are mixed and stirred at 50°C for 13 h (monitored by TLC). The reaction mixture is filtered rapidly through a small amount of SiOj with EtOAc as the eluent to remove inorganic salts and dibutyltellurium oxide. Preparative TLC with EtOAc/petroleum ether at 60-90°C (1 9) as the eluent yields 3-phenylpropenoate (160 mg (98%)). 

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