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2. To these reactants was added 50 mL of THF under argon, and the reaction mixture was refluxed for 134 h. After the reaction was cooled, the volatile components were remove in vacuo and the residue was extracted with copious amounts of pentane. The extract was concentrated to about 5 mL and kept in a freezer for 1 day, which allowed red-orange crystals for form. After filtration at -50 °C and washing with cold pentane, 0.36 g of crystalline 1 was obtained in 46% yield.
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