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A mixture containing phenyl hydrazine or hydrazine (5 mmol) and 1 (5 mmol) was sonicated in a 10 mL test tube for appropriate length of time (as indicated in Table 1) until TLC showed complete disappearance of the start- ing materials. In temperature controlled experiments, reac- tions were performed in a water bath at 25 ± 1 C. The reaction mixture was poured into ice–water mixture and the precipitates were collected by ?ltration. The pure prod- uct was obtained by recrystallization of the precipitates using ethanol and water. Products were identi?ed based on their melting point,H NMR,C NMR, and IR data. Known structures were veri?ed by comparison of their data with those reported in the literature [26]. |
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2楼2010-11-04 13:21:48
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