3,3,6,6-四甲基-9-对氯苯基-1,8-二氧代-2,3,4,5,6,7-六氢氧杂蒽的合成和晶体结构  

Synthesis and Crystal Structure of 3,3,6,6 tetramethyl-9-(4 chlorophenyl)-1,8- dioxo-2,3,4,5,6,7-hexahydroxanthene

作　　者：屠树江[1] 史达清[1] 姚昌盛[1] 赵长春[1] 马恒俊[1] 

机构地区：[1]徐州师范大学化学系,江苏徐州221009

出　　处：《Chinese Journal of Structural Chemistry》2001年第1期49-52,共4页结构化学（英文）

摘　　要：标题化合物C2 3H2 5O3Cl是由对氯苯甲醛与 5,5 二甲基 1 ,3环己二酮在乙二醇中反应而得。结构通过单晶X 射线衍射法测定 ,其晶体属于单斜晶系 ,空间群P2 1 /n ,a =6.0 4 8(1 ) ,b =1 9.543(3) ,c =1 7.42 0 (3) ,β =97.2 9(1 )° ,V =2 0 4 2 .2 (6) 3,Mr=384.90 ,Dc=1 2 52 g/cm3,Z =4,μ(MoKα) =2 .0 6cm- 1 ,F(0 0 0 ) =81 6。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最终的偏离因子为R =0 .0 39,Rw=0 .0 4 7。X 射线衍射分析表明 :平面 1 (C(8) -C(9) -C(1 9) )与平面 2 (C(1 0 ) -C(1 1 ) -C(1 2 ) )之间的两面角为1 6.2 4° ;平面 1与平面 3(C(7) -C(8) -C(9) )之间的两面角为 1 77.37° ;平面 1与平面 4(C(1 )-C(5) -C(6) )之间的两面角为 98.2 1°;平面 2与平面 3之间的两面角为 1 61 .1 2° ;平面 2与平面 4之间的两面角为 81 .98°;平面 3与平面 4之间的两面角为 79.1The title compound (C 17 H 19 NO 2) has been synthesized by reaction of benzaldehyde and 5,5 dimethyl 1,3 cyclohexamedione, isopropylidene malonate and ammonium acetate under microwave irradiation,and its structure was determined by single crystal X ray diffraction .The crystal is monoclinic, space group P2 1/a a=7.524(2),b=22.483(3),c=9.273(2) ,β=113.04(2)°,V=1443.7(5) 3,M r=269.34,D c =1.239g/cm 3, Z=4,μ (Mo Kα )=0.81cm -1 , F (000) =576. The structure was solved by direct methods, and refined by full matrix least square method to a final R=0.044 and R w =0.058. X ray analysis reveals that the dihedral angle between plane 1 C(12)～C(17) and plane 2 O(3)-C(9)-C(4)-C(5)-N(1) is 84.25°。

关 键 词：微波 干反应 合成 晶体结构 4-苯基-7 7-二甲基 

分 类 号：O626[理学—有机化学]