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33544467910
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note
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Silica gel-supported ammonium thiocyanate was prepared as follows. Silica gel (18.48 g) was added to a solution of ammonium thiocyanate (20 mmol 1.52 g) in dry acetonitrile (50 mL), and the mixture was stirred at room temperature for 30 min. The acetonitrile was removed under reduced pressure. The resulting reagent was dried in vacuo (15 mmHg) at room temperature for 3 h.
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24
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33544461703
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note
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4. The solvent was evaporated under reduced pressure to leave the crude product, which was purified by recrystallization (methanol).
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