【摘要】 多虑平类化合物在溶液体系中可能存在着构象交换过程,在其核磁共振图谱中出现的谱线展宽(包峰)或缺失现象增加了化合物结构解析的难度,甚至产生误导。该文以多虑平类化合物11-[(3-二甲基氨基)亚丙基]-6,11-二氢二苯并[b,e]氧杂-2-甲醛为样本,通过改变实验条件证明该化合物在几种溶液体系中均存在着构象交换。实验表明升温可以改善这类化合物的核磁共振测试效果,在80℃下获取的谱图信号清晰完整,信号展宽和缺失现象得到有效抑制。利用升温条件下获取的谱图,顺利实现了对11-[(3-二甲基氨基)亚丙基]-6,11-二氢二苯并[b,e]氧杂-2-甲醛的结构解析。更多还原

【Abstract】 In this work,NMR spectral characteristics of doxepin compounds were investigated with various experimental conditions, taking 11-( 3-dimethylaminopropylidene)-6,11-dihydro-dibenzo[b,e]oxepine-2-carbaldehyde( DP) as the testing sample. The conformation exchange of DP was confirmed. It was proved that the NMR spectral characteristics would depend on the experimental conditions,and the temperature would greatly affect the characteristics of the signals. Under the room temperature,the phenomena of signal broadening and missing were observed. As a result,the NMR signal assignment could not be accomplished. These phenomena could be improved with increase of temperature. The abnormal phenomena were effectively inhibited at 80 ℃. Finally,the complete assignment was presented and configuration was confirmed.更多还原