有机化学
有機化學
유궤화학
CHINESE JOURNAL OF ORGANIC CHEMISTRY
2001年
1期
49-52
,共4页
朱文峰%曾广怀%程华威%宋礼成
硃文峰%曾廣懷%程華威%宋禮成
주문봉%증엄부%정화위%송례성
μ3-S%μ3-Se%立方烷簇合物%官能团取代环戊二烯基%自组装反应
μ3-S%μ3-Se%立方烷簇閤物%官能糰取代環戊二烯基%自組裝反應
μ3-S%μ3-Se%립방완족합물%관능단취대배무이희기%자조장반응
通过(η5-C5H5)2Fe2(C O)4和硒粉在沸腾的甲苯中反应可制得含μ3-Se的立方烷簇合物(η5-C5H5)4 Fe4(μ3-Se)4 (1),而由(η5-RC5H4)2Cr2(CO )4S在甲苯中回流可制得含μ3-S的立方烷簇合物(η5-RC5H4)4Cr4(μ3 -S)4 (2,R=COMe;3,R=CO2Me)。企 图通过(η5-EtO2CC5H4)2Fe2(CO)4 (5)和硫黄制 备μ3-S立方烷簇合物(η5-EtO2CC5H4)4Fe4(μ3-S)4 ( 6)未获成功,其中5是由η5-EtO2CC5H4Fe(C O)2Na与η5-EtO2CC5H4Fe(CO)2I (4)缩合制得。新化合物1~5经元素分析,IR和1H NMR光谱表征。
通過(η5-C5H5)2Fe2(C O)4和硒粉在沸騰的甲苯中反應可製得含μ3-Se的立方烷簇閤物(η5-C5H5)4 Fe4(μ3-Se)4 (1),而由(η5-RC5H4)2Cr2(CO )4S在甲苯中迴流可製得含μ3-S的立方烷簇閤物(η5-RC5H4)4Cr4(μ3 -S)4 (2,R=COMe;3,R=CO2Me)。企 圖通過(η5-EtO2CC5H4)2Fe2(CO)4 (5)和硫黃製 備μ3-S立方烷簇閤物(η5-EtO2CC5H4)4Fe4(μ3-S)4 ( 6)未穫成功,其中5是由η5-EtO2CC5H4Fe(C O)2Na與η5-EtO2CC5H4Fe(CO)2I (4)縮閤製得。新化閤物1~5經元素分析,IR和1H NMR光譜錶徵。
통과(η5-C5H5)2Fe2(C O)4화서분재비등적갑분중반응가제득함μ3-Se적립방완족합물(η5-C5H5)4 Fe4(μ3-Se)4 (1),이유(η5-RC5H4)2Cr2(CO )4S재갑분중회류가제득함μ3-S적립방완족합물(η5-RC5H4)4Cr4(μ3 -S)4 (2,R=COMe;3,R=CO2Me)。기 도통과(η5-EtO2CC5H4)2Fe2(CO)4 (5)화류황제 비μ3-S립방완족합물(η5-EtO2CC5H4)4Fe4(μ3-S)4 ( 6)미획성공,기중5시유η5-EtO2CC5H4Fe(C O)2Na여η5-EtO2CC5H4Fe(CO)2I (4)축합제득。신화합물1~5경원소분석,IR화1H NMR광보표정。
A cubane-type cluster (η5-C5H5)4Fe4( μ3-Se)4 (1)was prepared by reaction of (η5-C5H5)2F e2(CO)4 with elemental selenium in refluxing toluene,whereas two cubane-ty pe clusters with a general formula (η5-RC5H4)4Cr4(μ3-S)4 (2, R=COMe; 3, R=CO2Me), were obtained by self-asse mb ly reaction of (η5-RC5H4)2Cr2(CO)4S in toluene at reflux. An attem pt to prepare cubane-type cluster (η5-EtO2CC5H4)4Fe4(μ3-S)4 was unsuccessful through reaction of elemental sulfur and (η5-EtO2CC5H 4)2Fe2(CO)4 (5) made from η5- EtO2CC5H4Fe(CO)2 Na and η5-EtO2CC5H4Fe(CO)2I (4). New compounds 1~5 have been characterized by elemental analysis, IR and 1H NMR spectroscopies.