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1942484170
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note
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2O (500 mL, 10 mmol/L) under vigorous stirring in ambient condition; a brown Cu sol was formed in several minutes. Second, 4mmol O,O′-di-n-octyl dithiophosphoric acid dissolved in 500-mL benzene was added to the sol and further stirred for 3 h, with the gradual transformation of the organic phase into dark red colour. Third, the organic phase was separated and evaporated at 80°C in a rotary evaporator to remove the solvent; then the organic layer was mixed with 100-mL acetone to allow the generation of brown precipitate. The precipitate was filtered after storing for several hours and washed with acetone for three times. Finally, the crude product was dissolved in 10-mL ether and precipitated with acetone again, to allow the generation of the target compound at a yield of copper 81%. Further purification of the product could be achieved by the chromatographic separation of the crude product in a silica gel column using petroleum ether/acetone (4:1) as the eluent. In this case a dark brown solid was obtained at a yield of 40%.
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1942484171
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8HDTP, 82.3.
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