合成化学
閤成化學
합성화학
CHINESE JOURNAL OF SYNTHETIC CHEMISTRY
2010年
2期
172-175
,共4页
王健春%乔良%陈振民%石远%武晶晶%何平
王健春%喬良%陳振民%石遠%武晶晶%何平
왕건춘%교량%진진민%석원%무정정%하평
二茂铁%1,1′-二茂铁二甲醛%咪唑%合成%晶体结构
二茂鐵%1,1′-二茂鐵二甲醛%咪唑%閤成%晶體結構
이무철%1,1′-이무철이갑철%미서%합성%정체결구
ferrocene%1,1′-diformylferrocene%imidazole%synthesis%crystal structure
1,1′-二茂铁二甲醛与烷基二酮反应合成了3种新型的1,1′-双(4,5-二烷基咪唑)二茂铁,其结构经~1H NMR, ~(13)C NMR, IR, ESI-MS及元素分析表征.1,1′-双(4,5-二苯基咪唑)二茂铁醋酸盐(1a′)的晶体结构经X-射线单晶衍射表征.1a′的晶体结构显示二茂铁的两个取代咪唑通过与醋酸的氢键作用形成顺式构型,探讨了顺式构型与反式构型的转化条件. 1a′属单钭晶系,C2/c空间群,晶胞参数: a＝15.832(4), b=19.255(4) (A), c＝14.781(4) (A), β=121.837(3)°, V＝3828.0(15) (A)~3, Z＝4, F(000)＝1 687, Dc=1.395 g·cm~(-3), Mr＝804.07.
1,1′-二茂鐵二甲醛與烷基二酮反應閤成瞭3種新型的1,1′-雙(4,5-二烷基咪唑)二茂鐵,其結構經~1H NMR, ~(13)C NMR, IR, ESI-MS及元素分析錶徵.1,1′-雙(4,5-二苯基咪唑)二茂鐵醋痠鹽(1a′)的晶體結構經X-射線單晶衍射錶徵.1a′的晶體結構顯示二茂鐵的兩箇取代咪唑通過與醋痠的氫鍵作用形成順式構型,探討瞭順式構型與反式構型的轉化條件. 1a′屬單鈄晶繫,C2/c空間群,晶胞參數: a＝15.832(4), b=19.255(4) (A), c＝14.781(4) (A), β=121.837(3)°, V＝3828.0(15) (A)~3, Z＝4, F(000)＝1 687, Dc=1.395 g·cm~(-3), Mr＝804.07.
1,1′-이무철이갑철여완기이동반응합성료3충신형적1,1′-쌍(4,5-이완기미서)이무철,기결구경~1H NMR, ~(13)C NMR, IR, ESI-MS급원소분석표정.1,1′-쌍(4,5-이분기미서)이무철작산염(1a′)적정체결구경X-사선단정연사표정.1a′적정체결구현시이무철적량개취대미서통과여작산적경건작용형성순식구형,탐토료순식구형여반식구형적전화조건. 1a′속단두정계,C2/c공간군,정포삼수: a＝15.832(4), b=19.255(4) (A), c＝14.781(4) (A), β=121.837(3)°, V＝3828.0(15) (A)~3, Z＝4, F(000)＝1 687, Dc=1.395 g·cm~(-3), Mr＝804.07.
Three novel 1,1′-bis(4,5-dialkyl)imidazole ferrocenes were synthesized by the reaction of 1,1′-diformylferrocene with alkyldiketones. The structures were characterized by ~1H NMR, ~(13)C NMR, IR, ESI-MS and elemental analysis. The crystal structure of 1,1′-ferrocenyl-bis(4,5-diphenyl) imidazolium acetate(1a′) was studied by X-ray diffraction. The results showed that two imidazole rings are cis-configuration by hydrogen bond between imidazoles and acetic acid. Transformation conditions of cis- and trans-configurations were studied. 1a′ belongs to monoclinic, space group C2/c with a＝15.832(4) , b=19.255(4) (A), c＝14.781(4) (A) , β=121.837(3)°, V＝3828.0(15) (A)~3, Z＝4, F(000)＝1 687, Dc=1.395 g·cm~(-3), Mr＝804.07.
