Process for producing metallocenes
A kind of technology of metallocene, alkali metal alkoxide, be used in the intermediate field of synthesizing described metallocene
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example 1
[0091] Reaction Step (a) Synthesis of 2,2-bis-indenylpropane
[0092]All manipulations were performed under an inert gas atmosphere (argon). A 2 L volume double wall reactor was charged with DMSO (100 mL), NaOMe (0.9 g, 0.02 mol) and indene (40 g, 0.33 mol) and stirred at 20° C. for 30 minutes. The reactor was cooled to 10 °C. Then, acetone (9.7 g, 0.17 mol) was added over 15 minutes keeping the reactor temperature below 20°C (exothermic reaction). The reaction mixture was then stirred at 40 °C for 2 h and at room temperature overnight until the reaction was complete (6,6-dimethylfulvene <1% as judged by GC). 100 g of water was added at 10° C. and stirred for 30 minutes, then methyl tert-butyl ether (MTBE; 236 g) was added to the reaction mixture. The mixture was stirred for another 30 minutes at room temperature.
[0093] The two phases were separated, the aqueous phase was extracted again with MTBE, and the combined organic phases were washed with saturated aqueous NaCl...
example 2
[0102] Example 2 was performed the same as Example 1, except that the bridging benzophenone (O=CPh 2 ; 15.2g, 0.08mol) instead, and the amount of NaOMe was doubled. The product was dried in vacuo yielding 35.5 g (0.064 mol, 80.1% i.y) of fine orange to red crystals.
example 3
[0104] Example 3 was performed the same as Example 1, except that DMF (dimethylformamide) was used as the solvent as shown in Table 1. The product was dried in vacuo yielding 20.0 g (0.073 mol, 44.2%) of fine white crystals.
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