以乙腈作溶剂,苄基溴和二苯胺在叔丁醇钾的催化下,可以直接合成得到N,N-二苯基苄叔胺类化合物,产率60.2%~81.4%。产物经1 H NMR、13 C NMR和GC-MS确证。得出合成N,N-二苯基叔胺最优化条件为n（苄基溴）∶n（二苯胺）∶n（叔丁醇钾）=1.5...以乙腈作溶剂,苄基溴和二苯胺在叔丁醇钾的催化下,可以直接合成得到N,N-二苯基苄叔胺类化合物,产率60.2%~81.4%。产物经1 H NMR、13 C NMR和GC-MS确证。得出合成N,N-二苯基叔胺最优化条件为n（苄基溴）∶n（二苯胺）∶n（叔丁醇钾）=1.5∶1∶1,以乙腈为溶剂,室温下反应12h。该方法具有反应条件温和,操作简单,产率较高等优点。展开更多
C 60 /C 70 mixture reacts with hydrazine hydrate catalysed by tetrabutylammonium bromide (TBAB) in the presence of air to afford fullerene hydrazine derivatives C 60 (OH) n(NHNH 2) n and C 70 (OH) n(NHNH 2) n,whi...C 60 /C 70 mixture reacts with hydrazine hydrate catalysed by tetrabutylammonium bromide (TBAB) in the presence of air to afford fullerene hydrazine derivatives C 60 (OH) n(NHNH 2) n and C 70 (OH) n(NHNH 2) n,which are characterized by means of MS and FTIR.A possible reaction mechanism is discussed.展开更多
通过芳基硫脲1a^g与3-氯-2,4-戊二酮2环合得到2-芳氨基-4-甲基-5-乙酰基噻唑3a^g,再与肼基甲酸甲酯4进行缩合反应得到目标产物。以5e为例,分别对反应时间、催化剂种类及物质的量比进行了试验,最佳的缩合反应条件是:反应时间6h,催化剂用...通过芳基硫脲1a^g与3-氯-2,4-戊二酮2环合得到2-芳氨基-4-甲基-5-乙酰基噻唑3a^g,再与肼基甲酸甲酯4进行缩合反应得到目标产物。以5e为例,分别对反应时间、催化剂种类及物质的量比进行了试验,最佳的缩合反应条件是:反应时间6h,催化剂用浓盐酸,物质的量比1∶1.1,收率70.9%。合成得到7个目标产物2-[1-(2-芳氨基-4-甲基噻唑-5)-乙缩醛]肼基甲酸甲酯5a^g,目标化合物结构经IR、1 H NMR、MS和元素分析确证。采用MTT法对MCF-7和SMMC-7721人肿瘤细胞株进行体外抗肿瘤活性测试,结果发现此类化合物活性较弱,化合物5f有一定的抗肿瘤活性。展开更多
The crystals of the title compound C_(15)H_(17)N_2O_2PS were obtained by re crystallizing from ether-methanol solution. It belongs to the orthorhombic system, space group Pbca with a= 9. 255(1) , b= 17.189(8) , c =20....The crystals of the title compound C_(15)H_(17)N_2O_2PS were obtained by re crystallizing from ether-methanol solution. It belongs to the orthorhombic system, space group Pbca with a= 9. 255(1) , b= 17.189(8) , c =20. 446(4)A, V=3252.6 (7) A￣3, D_c=1. 31 g/cm￣3,Z= 8, μ(CuKa)=26. 87 cm-1, F(000)=1344. The structure was refined to R=0. 053, R_w=0. 055 for 1299 observed reflections (I≥3σ(I)). In the molecule P atom adopts distorted tetrahedral configuration.The bond (II)distances of P-O, P-N and P-C are 1.605(1) A, 1. 657(1) A 1. 801(1)A,(III)respectively. The X-ray crystallographic analysis demonstrates that there are intramolecular and intermolecular hydrogen bonds in the structure.展开更多
文摘以乙腈作溶剂,苄基溴和二苯胺在叔丁醇钾的催化下,可以直接合成得到N,N-二苯基苄叔胺类化合物,产率60.2%~81.4%。产物经1 H NMR、13 C NMR和GC-MS确证。得出合成N,N-二苯基叔胺最优化条件为n（苄基溴）∶n（二苯胺）∶n（叔丁醇钾）=1.5∶1∶1,以乙腈为溶剂,室温下反应12h。该方法具有反应条件温和,操作简单,产率较高等优点。
文摘C 60 /C 70 mixture reacts with hydrazine hydrate catalysed by tetrabutylammonium bromide (TBAB) in the presence of air to afford fullerene hydrazine derivatives C 60 (OH) n(NHNH 2) n and C 70 (OH) n(NHNH 2) n,which are characterized by means of MS and FTIR.A possible reaction mechanism is discussed.
文摘通过芳基硫脲1a^g与3-氯-2,4-戊二酮2环合得到2-芳氨基-4-甲基-5-乙酰基噻唑3a^g,再与肼基甲酸甲酯4进行缩合反应得到目标产物。以5e为例,分别对反应时间、催化剂种类及物质的量比进行了试验,最佳的缩合反应条件是:反应时间6h,催化剂用浓盐酸,物质的量比1∶1.1,收率70.9%。合成得到7个目标产物2-[1-(2-芳氨基-4-甲基噻唑-5)-乙缩醛]肼基甲酸甲酯5a^g,目标化合物结构经IR、1 H NMR、MS和元素分析确证。采用MTT法对MCF-7和SMMC-7721人肿瘤细胞株进行体外抗肿瘤活性测试,结果发现此类化合物活性较弱,化合物5f有一定的抗肿瘤活性。
文摘The crystals of the title compound C_(15)H_(17)N_2O_2PS were obtained by re crystallizing from ether-methanol solution. It belongs to the orthorhombic system, space group Pbca with a= 9. 255(1) , b= 17.189(8) , c =20. 446(4)A, V=3252.6 (7) A￣3, D_c=1. 31 g/cm￣3,Z= 8, μ(CuKa)=26. 87 cm-1, F(000)=1344. The structure was refined to R=0. 053, R_w=0. 055 for 1299 observed reflections (I≥3σ(I)). In the molecule P atom adopts distorted tetrahedral configuration.The bond (II)distances of P-O, P-N and P-C are 1.605(1) A, 1. 657(1) A 1. 801(1)A,(III)respectively. The X-ray crystallographic analysis demonstrates that there are intramolecular and intermolecular hydrogen bonds in the structure.
