摘要
某固体化合物极易溶于水但未能制得其单晶．为测定其结构可充分发挥ＮＭＲ的特长．利用ＮＭＲ的多种技术，包括常规￣１Ｈ谱、￣（１３）Ｃ谱，一维、二维谱，确定脂肪链Ｘ－ＣＨ＿２－ＣＨ＿２－ＣＨ＿２－Ｙ与芳香基团Ｙ的存在；利用￣（１３）Ｃ－￣１Ｈ长程耦合相关谱（用反相探头）可确定脂肪链与芳香基团间的联接关系，于是立即可确定该物的有机主体骨架应为Ｘ－ＣＨ＿２－ＣＨ＿２－ＣＨ＿２－Ｙ．从ＩＲ谱得知该物除存在Ｃ－Ｎ基团外，还存在－ＳＯ＿３－基团等．从元素成分分析和Ｍ８谱，包括ＦＡＢ－ＭＳ谱等分析结果，最终推断该固体化合物为丙磺酸吡啶内盐，它的分子结构应为：
An unknown white solid compound is very soluble in water．Its single crystal isnot obtained now．The NMR technique plays an important role in determining itsstructure．From the routine ~1H NMR spectrum（Fig．1），^(13)C NMR spectrum，decouplingwithout NOE ^(13)C NMR spectrum，off－resonace ^(13)C NMR spectrum，（Fig．3），~1H－~1HCOSY spectrum（Fig．2），and 13C－~1H correlated 2D spectrum （Fig．4），it proves thatthere are an alkylchain X－CH_2－CH_2－CH_2－Y and an aromatic group in thiscompound．^(13)C－~1H correlated spectrum via long range couplings （in inverse probe）（Fig．5）may determine how to connect between the chain and the group．So its mainskeletal must be X－CH_2－CH_2－CH_2．IR spectrum（Fig．6），shows us theexistance of the －SO_3－ group．From the results of element analysis and MS spec-trum，including FAB－MS spectrum（Fig．7 and 8），It was finally judged that the molecularstructure of this compound should be the internal salt of pyridinium－N－propane－sulfonic acid．Its structural formula is
出处
《波谱学杂志》
CAS
CSCD
1995年第3期309-314,共6页
Chinese Journal of Magnetic Resonance
关键词
结构分析
NMR
红外谱
快原子轰击质谱
Structural analysis， Internal salt of pyridinium－N－propane－sulfonic acid，1D and2D NMR，FT－IR，FAB－MS
