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594306435

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594306435(½ð±Ò+10, ·­ÒëEPI+1): ̫ллÁË 2011-04-06 16:47:53
Compound 1 was dissolved in triethyl phosphite and reacted for an hour at 40 degree C. Then the solution was cooled down, and the excess triethyl phosphite was separated by distillation under reduced pressure. The resulting product was directly dissolved in absolute DMF, then, NaH and aromatic aldehyde were added and stirred for 1 hr at room temperature and another 1 hr at 30 ¡ã C, finally, 5mL 5%NaOH was added into the solution. The whole reaction process was monitored by TLC. After the reaction, the solution was cooled down and an acidification was carried out with 1mmol/L HCl, a solid rough product x was obtained by filtration. The pure product was prepared by recrystallization of compound with ethanol and the remaining compounds kept unchanged.
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