Olefin metathesis catalyst containing tungsten fluorine bonds
a technology of tungsten fluorine bond and catalyst, which is applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, bulk chemical production, etc., can solve the problems of steam cracking, insufficient propylene, and complex combination of reaction and gas recovery system
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example 1
Synthesis of W═OF(CH2CMe3)3
[0037]The synthesis of [W═O(CH2CMe3)3F] was carried out according to the following reaction.
W═O(CH2CMe3)3Cl was synthesized by the literature procedure (Schrock et. al. , J. AM. CHEM. SOC. 1984, 106, 6305-10). [W═O(CH2CMe3)3Cl] (1.5 g,) and AgBF4 (0.65 g) were stirred in 20 mL of toluene for one hour at room temperature. The reaction mixture was filtered to remove the insoluble AgCl, and NEt3 (1.1 mL) was added to remove the BF3 moiety by precipitation as BF3.N(C2H5)3. The resulting solution was stirred for 16 h at room temperature and then filtered over celite. The solvent was then removed under vacuum to provide a white solid which was sublimed at 60° C. under reduced pressure (3.10-5 Torr) to yield 1.13 g of product. The product was analyzed and found to contain 41.47% C; 7.89% H and 4.72% F which agrees well with calculated percentages for C15H33OFW of 41.69% C; 7.69% H and 4.42% F.
example 2
Synthesis of W(NPh)F(CH2CMe3)3
[0038]W(NPh)F(CH2CMe3)3 was synthesized by reaction of WOCl4 with C6H5NCO, followed by alkylation with neopentyl magnesium chloride as shown below.
[0039]Freshly distilled phenylisocyanate (3.214 g) was added to a suspension of [W═OCl4] (9.000 g) in 200 mL of heptane. This mixture was heated at reflux temperature for 4 days to provide a dark brown precipitate. The solvent was removed under vacuum and Et2O (20mL) was added resulting in a green solution mixture which was filtered to remove the insoluble impurities and Et2O was then removed under vacuum producing a powder of dark green crystals of [W═N(C6H5)Cl4].(Et2O). A solution of 10.6 g [W═N(C6H5)Cl4].(Et2O) in toluene was prepared and stirred rapidly. This solution was cooled to −78° C. and to it there were added (dropwise) 30 mL of a 2.17 M ether solution of neopentylmagnesium chloride. The mixture was warmed up slowly to room temperature with continuous stirring at which point the solvent was remove...
example 3
Synthesis of WOF(CH2CMe3)3 / SiO2
[0041]A mixture of the product of Example 1 [WO(CH2CMe3)3F] (500 mg) in pentane (10 mL) and SiO2-(700) (2 g) was stirred at 25° C. overnight. After filtration, the solid was washed 5 times with pentane and all volatile compounds were condensed into another reactor (of known volume) in order to quantify neopentane evolved during grafting. The resulting white powder was dried under vacuum (10−5 Torr). Analysis by gas chromatography indicated the formation of 290 μmol of neopentane during the grafting (1.0±0.1 NpH / W). Elemental analysis showed: W 4.43 wt-%; C 3.27 wt-%.
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