Abstract
So far, few microclusters containing vanadium have been described in the literature. In this report, the synthesis protocol for the preparation of oxovanadium (IV) microclusters with 2-phenylpyridine is shown for the first time. Moreover, the crystal structure of these microclusters is also studied through the use of X-rays. The morphology of the prepared crystals is investigated using a field-emission Scanning Electron Microscope (SEM). The new compound, after activation by modified methylaluminoxane as the catalytic system, is investigated regarding the oligomerizations of 3-buten-1-ol, 2-chloro-2-propen-1-ol, allyl alcohol, and 2,3-dibromo-2-propen-1-ol. The products of oligomerization are tested by the TG-FTIR and MALDI-TOF-MS methods. Moreover, the values of catalytic activities for the new oxovanadium(IV) microclusters with 2-phenylpyridine are determined for the 3-buten-1-ol, 2-chloro-2-propen-1-ol, allyl alcohol, and 2,3-dibromo-2-propen-1-ol oligomerizations. Oxovanadium(IV) microclusters with 2-phenylpyridine are shown to be very highly active precatalysts for the oligomerization of allyl alcohol, 2,3-dibromo-2-propen-1-ol, and 3-buten-1-ol. However, in the case of 2-chloro-2-propen-1-ol oligomerization, the new microclusters are seen as highly active precatalysts.
Highlights
The metathesis of olefin has been known and used in organic synthesis since the middle of the twentieth century [1,2]
The reagents used for the synthesis of oxovanadium(IV) microclusters with 2-phenylpyridine were as follows: vanadyl acetylacetonate (98% purity), oxydiacetic acid (98% purity), and 2-phenylpyridine (98% purity)
The π-stacked columns formed by one 2-pheny4lpoifri1d2ine molecule and three 2-phenylpyridine cations were connected with these layers via strong N– H···O(water), O(water)–H··· O(cluster), and O(water)–H···N(pyridine) hydrogen bonds and weak C(pyridine)–H···O(cluster) hydrogen bonds to form a 3D framework structure (Figure 3, Table 2)
Summary
The metathesis of olefin has been known and used in organic synthesis since the middle of the twentieth century [1,2]. The following systems were used as catalysts: TiCl4/AlEt3, MoCl5/AlEt3, and WCl6/AlEt3 [7] Due to their low cost and simple synthesis, they have played an important role in the industrial use of olefin metathesis—e.g., in the Shell Higher Olefin Process (SHOP) [8]. These have allowed for the efficient course of ringopening metathesis polymerization (ROMP) and cross-metathesis (CM). The synthesis of new, stable complex compounds catalyzing the olefin oligomerization and polymerization reaction, as well as proposing their mechanisms, is a challenge for the generation of scientists Many catalytic systems, both homogeneous and heterogeneous, can be used to initiate olefin metathesis [13]. Mainly organic compounds are used as ligands—e.g., pyridine, lactones, proline derivatives, quinoline, 2,2 -bipyridine, pyrazine, or organophosphorus compounds [16,17,18,19,20,21,22]
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