2,4-二羟基-3,5-二氯苯乙酮的微波合成及晶体结构

Microwave synthesis and crystal structure of 2,4-dihydroxy-3,5-dichloroacetophenone

以2,4-二羟基苯乙酮、氯酸钾和盐酸为原料,在微波辅助作用下,合成了2,4-二羟基-3,5-二氯苯乙酮,研究了溶剂的用量、反应辐射功率和反应时间对产物的影响.利用核磁共振波谱、红外光谱及单晶X射线法对目标化合物进行表征.研究表明,该化合物为单斜晶系,空间群为P21/c,晶体学参数:a=0.800 6(4)nm,b=1.499 2(8)nm,c=0.729 5(4)nm;α=γ=90°,β=95.506(6)°;F(000)=448,Z=4,V=0.871 6(8)nm3,Dc=1.684g·cm-3,Mr=221.03.最终结构偏离因子R=0.051 6,Rw=0.150 8;S=1.121.最终差值电子密度的最大值和最小值分别为509nm-3和-580nm-3.

The title compound,2 ,4-dihydroxy-3 ,5-dichloroacetophenone,has been designed and microwave synthe-sized by 2 ,4-dihydroxyacetophenone,KClO3 and HCl.The influence of the solvent dosage,reaction time and micro-wave radiation power on the synthesis has been studied.The structure was determined by 1 HNMR,IR and single X-ray crystallography study.The title compoud C8 H6 Cl2 O3 crystallizes in the monoclinic space group P21/c with the cell parameters a= 0. 800 6(4)nm,b= 1. 499 2(8)nm,c= 0. 729 5(4)nm,α=γ= 90°,β= 95. 506(6)°,F(000)=448,Z= 4,V= 0. 871 6(8)nm3 ,Dc= 1. 684 g·cm-3 ,Mr= 221. 03.R= 0. 051 6,Rw= 0. 150 8,S= 1. 121.The lar-gest difference in peak and hole are 509 nm-3 and -580 nm-3 .