کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
5219063 | 1383346 | 2012 | 7 صفحه PDF | دانلود رایگان |
![عکس صفحه اول مقاله: Measurement and optimization of organic chemical reaction yields by GC-MS with supersonic molecular beams Measurement and optimization of organic chemical reaction yields by GC-MS with supersonic molecular beams](/preview/png/5219063.png)
A new type of gas chromatograph mass spectrometer (GC-MS) was used for semi-online monitoring of organic chemical reactions for their yield optimization, mechanism elucidation, and for obtaining information on the reaction products identity and purity. It was used with reaction mixtures without prior separation and purification as needed for NMR, thereby saving time and effort. Our unique GC-MS named 5975-SMB Supersonic GC-MS is based on GC interface with the MS with supersonic molecular beams (SMB) and on ionization of the sample molecules during their axial flight through an open electron ionization ion source as vibrationally cold molecules. GC-MS with SMB is demonstrated to significantly extend the range of compounds amenable for analysis, practically always giving molecular ions, enabling effective fast GC-MS analysis, and providing elemental formulas via isotope abundance analysis with unit mass resolution quadrupole MS. In addition, it uniquely provides uniform response to all compounds, a feature, which is vital for the measurement of chemical reaction yields. In this manuscript, four different organic synthetic reactions were studied and are described. Based on the collected data, we were able to better understand how the reaction conditions should be optimized in order to maximize the yields and purity of target products. Consequently, we propose that GC-MS with SMB can serve as a novel tool for the fast optimization of chemical reactions.
Journal: Tetrahedron - Volume 68, Issue 29, 22 July 2012, Pages 5793-5799