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note
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2 (4 × 1865 mL), and the combined organic layers were concentrated to an oil. Addition of 135 mL of EtOH resulted in the crystallization of 2 as a light yellow solid, which was then washed with cold EtOH (2 × 50 mL), filtered, and dried to give 2 (56.64 g, 377 mmol) in 38.5% yield. The resultant filtrate was concentrated to a slurry, filtered, washed with EtOH (3 × 20 mL), and dried to give additional 2 (13.93 g, 93 mmol, 9.5% yield), which had a lower potency.
-
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20
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84889524173
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note
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13C NMR, IR, and elemental analysis data were obtained for all reaction products.
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84889517522
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note
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2O/MeCN; 2:1 (2 × 1.5 L), MeCN (2 × 1.5 L), and then dried in vacuo at 50-60 °C overnight to give 7b (425 g, 1.42 mol) in 94% yield.
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