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邻氯苯甲醛与季戊四醇反应得到中间体5,5-二(羟甲基)-2-(2-氯苯基)-1,3-二氧六环(1),1再与环己酮反应生成12-(2-氯苯基)-7,11,13,16-四氧杂二螺[5.2.5.2]十六烷(2).反之,先用环己酮与季戊四醇反应生成9,9-二(羟甲基)-7,11-二氧杂螺[5.5]十一烷(3),3再与邻氯苯甲醛反应也可生成标题化合物2.化合物1和2的结构用X射线单晶衍射、元素分析和核磁共振氢谱进行了确定.X射线单晶衍射晶体结构表明化合物1属单斜晶系,空间群为P2(1)/n,晶体学参数:a=0.56768(15)nm,b=0.9807(3)nm,c=2.1785(6)nm,a=90°,β=90.204(4)°,γ=90°,V=1.2128(5)nm3,Z=4,Dc=1.417Mg/m3,μ=0.315 mm-1,F(000)=544.化合物2也属于单斜晶系,空间群为C2/c,晶体学参数:a=1.5894(5)nm,b=1.5704(4)nm,c=2.8369(9)nm,a=90°,β=101.103(5)°,γ=90°,V=6.948(4)nm3,Z=16,Dc=1.296 Mg/m3,μ=0.237mm-1,F(000)=2880.
The reaction of o-chlorobenzaldehyde with pentaerythritol gives the intermediate 5,5-bis (hydroxymethyl) -2- (2-chlorophenyl) -1,3-dioxane (1) 12- (2-chlorophenyl) -7,11,13,16-tetraoxadispiro [5.2.5.2] hexadecane (2) is produced, whereas cyclohexanone and pentaerythritol are first reacted to form 9,9 -bis (hydroxymethyl) -7,11-dioxaspiro [5.5] undecane (3), 3 followed by o-chlorobenzaldehyde also gave the title compound 2. The structures of compounds 1 and 2 were characterized by X-ray Single crystal diffraction, elemental analysis and 1H nuclear magnetic resonance spectroscopy were used to determine the crystal structure of X-ray single crystal.The crystal structure of X-ray single crystal diffraction showed that compound 1 belongs to the monoclinic system with space group P2 (1) / n and the crystallographic parameters: a = 0.56768 ) nm, b = 0.9807 (3) nm, c = 2.1785 (6) nm, a = 90 °, β = 90.204 (4) °, γ = 90 °, V = = 1.417Mg / m3, μ = 0.315 mm-1, F (000) = 544.Compound 2 also belongs to the monoclinic system with C2 / c space group and its crystallographic parameters are as follows: a = 1.5894 1.5704 nm, c = 2.8369 nm, a = 90 °, β = 101.103 (5) °, γ = 90 °, V = 6.948 nm3, Z = 16 and Dc = 1.296 Mg / m3 , μ = 0.237 mm-1, F (000) = 2880.