青海大学学报：自然科学版
青海大學學報：自然科學版
청해대학학보：자연과학판
Journal of Qinghai University(Natural Science)
2011年
6期
64-67
,共4页
ω-溴代苯乙酮%三苯基膦%四溴化碳%1,13,-三溴-2-苯基丙烯%合成
ω-溴代苯乙酮%三苯基膦%四溴化碳%1,13,-三溴-2-苯基丙烯%閤成
ω-추대분을동%삼분기련%사추화탄%1,13,-삼추-2-분기병희%합성
ω-bromoacetophenone%triphenylphosphine%carbon tetrahalide%1%1%3-tribromo-2-phenylpropylene%synthesis
以苯乙酮为原料,经溴化反应得到ω-溴代苯乙酮,随后与三苯基膦、四溴化碳三组分一锅法合成1,13,-三溴-2-苯基丙烯。重点考察了三组分一锅法反应中反应溶剂、反应温度和反应时间等对产物收率的影响。获得较佳合成条件：n（ω-溴代苯乙酮）：n（三苯基膦）：n（四溴化碳）=1︰2.2︰1,反应介质为二氯甲烷,反应温度0℃,反应时间30 min,产物收率达82.7%。并通过红外光谱（FT-IR）和核磁共振波谱（1 H NMR1,3 C NMR）对产物结构进行了表征。
以苯乙酮為原料,經溴化反應得到ω-溴代苯乙酮,隨後與三苯基膦、四溴化碳三組分一鍋法閤成1,13,-三溴-2-苯基丙烯。重點攷察瞭三組分一鍋法反應中反應溶劑、反應溫度和反應時間等對產物收率的影響。穫得較佳閤成條件：n（ω-溴代苯乙酮）：n（三苯基膦）：n（四溴化碳）=1︰2.2︰1,反應介質為二氯甲烷,反應溫度0℃,反應時間30 min,產物收率達82.7%。併通過紅外光譜（FT-IR）和覈磁共振波譜（1 H NMR1,3 C NMR）對產物結構進行瞭錶徵。
이분을동위원료,경추화반응득도ω-추대분을동,수후여삼분기련、사추화탄삼조분일과법합성1,13,-삼추-2-분기병희。중점고찰료삼조분일과법반응중반응용제、반응온도화반응시간등대산물수솔적영향。획득교가합성조건：n（ω-추대분을동）：n（삼분기련）：n（사추화탄）=1︰2.2︰1,반응개질위이록갑완,반응온도0℃,반응시간30 min,산물수솔체82.7%。병통과홍외광보（FT-IR）화핵자공진파보（1 H NMR1,3 C NMR）대산물결구진행료표정。
1,1,3-tribromo-2-phenylpropylene was synthesized from ω-bromoacetophenone,triphenylphosphine and carbon tetrahalide.Firstly,the reaction of acetophenone and bromine the ω-dibromoacetophenone.Then,1,1,3-tribromo-2-phenylpropylene was obtained by the one-pot three-component reactions of ω-bromoacetophenone,triphenylphosphine and carbon tetrahalides.The effects of the reaction material ratio,temperature and time on the yield of the product were investigated.The optimal reaction conditions were obtained： ratio of ω-bromoacetophenone to triphenylphosphine and carbon tetrahalides is 1︰2.2︰1,the reaction temperature 0 ℃,the reation time is 30 min.The yield under this optimum reaction conditions was up to 82.7%.The structure of the target product was confirmed by FTIR,1H NMR and 13C NMR.
