摘要
报道了一种用5-硝基-2-胺基苯甲腈为原料,在二氯化锌催化下与环酮反应环化合成3,1-苯并噁嗪类化合物的新方法,并用此方法合成了6-硝基-1,2-二氢-2,2-(1,5-亚戊基)-4-亚胺-4H-3,1-苯并噁嗪(4a).产物经元素分析、红外光谱、核磁共振氢谱和碳谱进行了表征,用X射线单晶衍射法测定了其晶体结构.晶体属单斜晶系,P21/c空间群,a=0.66339(13)nm,b=2.5329(5)nm,c=0.73756(15)nm,β=91.85(3)°,V=1.2387(4)nm3,Z=4,Dc=1.401g/cm3,F(000)=552,μ=0.102mm-1,R=0.0994,wR=0.3001.
A new and efficient method for the synthesis of 3,1-benzoxazine compounds by direct cyclocondensation of 5-nitro-2-cyanoaniline with cyclic ketones using zinc chloride as catalyst was reported. Using this method, 6-nitro-1,2-dihydro-2,2-(1,5-pentylene)-4-imino-4H-3,1-benzoxazine (4a) was synthesized with its structure determined by elemental analysis, IR, 1H NMR, 13C NMR and X-ray single crystal diffraction analysis. Crystal data: monoclinic, space group: P21/c, a=0.66339(13) nm, b=2.5329(5) nm, c= 0.73756(15) nm, β=91.85(3)°, V= 1.2387(4) nm^3, Z=4, De= 1.401 g/cm^3, F(000)=552, μ =0.102 mm^-1, R=0.0994, wR=0.3001.
出处
《有机化学》
SCIE
CAS
CSCD
北大核心
2006年第7期928-932,共5页
Chinese Journal of Organic Chemistry