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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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簡(jiǎn)單 將5mmol的水合肼或者苯肼與1mmol 1的混合物放入10ml試管中超聲適當(dāng)?shù)臅r(shí)間(在表1中描述的),直到TLC監(jiān)測(cè)原料完全消失。實(shí)驗(yàn)過程中水浴的溫度控制在 25 ± 1 C。反應(yīng)完全后將反應(yīng)液倒入冰水中,過濾并收集析出的沉淀物,經(jīng)過乙醇和水混合溶劑重結(jié)晶得到純的產(chǎn)品,產(chǎn)品通過熔點(diǎn)測(cè)定、H NMR,C NMR, and IR 確認(rèn)。通過對(duì)比文獻(xiàn)【26】中報(bào)道的數(shù)據(jù)確認(rèn)了這種已知產(chǎn)品的結(jié)構(gòu)。 |

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