2-氟-5-[(4-氧代-3,4-二氢二氮杂萘-1-基)甲基]苯甲酸是合成奥拉帕尼的关键中间体。以邻羧基苯甲醛为原料,与亚磷酸二甲酯反应得到磷叶立德,再与2-氟-5-甲酰基苯甲酸进行WittigHorner反应、环合反应得到目标化合物,并对各步反应条件进...2-氟-5-[(4-氧代-3,4-二氢二氮杂萘-1-基)甲基]苯甲酸是合成奥拉帕尼的关键中间体。以邻羧基苯甲醛为原料,与亚磷酸二甲酯反应得到磷叶立德,再与2-氟-5-甲酰基苯甲酸进行WittigHorner反应、环合反应得到目标化合物,并对各步反应条件进行了优化,三步反应总收率70.9%。目标化合物经(1 H NMR)和(MS)确证结构。展开更多
We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,...We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,IR spectra,1HNMR spectra,electronic spectra and TG-DTA thermal analysis,and its crystal structure has been determined.The compound belongs to triclinic system,space group P ī with the following crystallographic parameters:a=7.691（2）,b=10.505（5）,c=17.692（5）,α=105.52（3）°,β=90.09（3）°,γ=103.92（4）°,V=1333.5（8）3,DC=1.377g/cm3,F（000）=582,μ（Mo Kα）=0.631mm-1,Z=1,and final R=0.0752,wR=0.1957 for 2425 observed reflections（I>2σ（I））.The analytical results of crystal structure and spectroscopic properties show that a square planar complex cation [Ni（hmta）]2+ is formed by coordination of four nitrogen atoms of ligand hmta to Ni（Ⅱ）.There isn’t interaction of Ni（Ⅱ） with sulfur atom of (2—C10H7O)2PSS-anion,but there are three N-H…S hydrogen bonds between [Ni（hmta）]2+ complex cation and(2—C10H7O)2PSS-anion in the compound.展开更多
文摘2-氟-5-[(4-氧代-3,4-二氢二氮杂萘-1-基)甲基]苯甲酸是合成奥拉帕尼的关键中间体。以邻羧基苯甲醛为原料,与亚磷酸二甲酯反应得到磷叶立德,再与2-氟-5-甲酰基苯甲酸进行WittigHorner反应、环合反应得到目标化合物,并对各步反应条件进行了优化,三步反应总收率70.9%。目标化合物经(1 H NMR)和(MS)确证结构。
文摘We reported the synthesis of [Ni（hmta）][SSP(OC10H7-2)2]2(where hmta is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane,and 2-C10H7O-is 2-nathphthyloxy).The complex is characterized by elemental analysis,IR spectra,1HNMR spectra,electronic spectra and TG-DTA thermal analysis,and its crystal structure has been determined.The compound belongs to triclinic system,space group P ī with the following crystallographic parameters:a=7.691（2）,b=10.505（5）,c=17.692（5）,α=105.52（3）°,β=90.09（3）°,γ=103.92（4）°,V=1333.5（8）3,DC=1.377g/cm3,F（000）=582,μ（Mo Kα）=0.631mm-1,Z=1,and final R=0.0752,wR=0.1957 for 2425 observed reflections（I>2σ（I））.The analytical results of crystal structure and spectroscopic properties show that a square planar complex cation [Ni（hmta）]2+ is formed by coordination of four nitrogen atoms of ligand hmta to Ni（Ⅱ）.There isn’t interaction of Ni（Ⅱ） with sulfur atom of (2—C10H7O)2PSS-anion,but there are three N-H…S hydrogen bonds between [Ni（hmta）]2+ complex cation and(2—C10H7O)2PSS-anion in the compound.
