A Quantitative NMR Method for Silyllithium Analysis

Synlett ◽  
2017 ◽  
Vol 28 (18) ◽  
pp. 2449-2452
Author(s):  
Scott Sieburth ◽  
Yingjian Bo

A rapid and extremely simple method for silyl anion analysis is presented. The progress of silyllithium reagent preparation can be determined by quenching an aliquot with neat chloro(trimethyl)silane, evaporation, dilution with CDCl3, and direct proton NMR analysis. This procedure is fast, simple, and allows for identification and relative quantification of the starting reagent, intermediates, and the silyllithium product.

Talanta ◽  
2021 ◽  
Vol 231 ◽  
pp. 122355
Author(s):  
Timothy J. Trinklein ◽  
Malati Thapa ◽  
Lexie A. Lanphere ◽  
John A. Frost ◽  
Sandra M. Koresch ◽  
...  

1994 ◽  
Vol 35 (11) ◽  
pp. 1925-1931
Author(s):  
R K Adosraku ◽  
G T Choi ◽  
V Constantinou-Kokotos ◽  
M M Anderson ◽  
W A Gibbons

2006 ◽  
Vol 103 (32) ◽  
pp. 11904-11909 ◽  
Author(s):  
P. Selenko ◽  
Z. Serber ◽  
B. Gadea ◽  
J. Ruderman ◽  
G. Wagner

1984 ◽  
Vol 121 (3) ◽  
pp. 1021-1026 ◽  
Author(s):  
Kofen Lai ◽  
Dinesh O. Shah ◽  
Eugene DeRose ◽  
David G. Gorenstein

2012 ◽  
Vol 66 (5) ◽  
pp. 1000-1006 ◽  
Author(s):  
Elisabeth Linton ◽  
Asif Rahman ◽  
Sridhar Viamajala ◽  
Ronald C. Sims ◽  
Charles D. Miller

In this study, a proton nuclear magnetic resonance (1H NMR) method was developed to quantitatively analyze polyhydroxyalkanoate (PHA) content in Cupriavidus necator H16, Azotobacter vinelandii AvOP, and mixed microbial cultures from the effluent of an agricultural waste treatment anaerobic digester. In contrast to previous methods, a single-step PHA extractive method using deuterated chloroform was established, thereby facilitating direct 1H NMR analysis. The accuracy of the method was verified through comparison with well-established gas chromatography (GC) methanolysis techniques. Nile blue fluorescence staining was also carried out to serve as an independent and qualitative indicator of intracellular PHA content. The results indicate that the 1H NMR method is appropriate for rapid and non-destructive quantification of overall PHA content and determination of PHA copolymer composition in a variety of cultures. Notably, this technique was effective in measuring PHA content in full-strength waste samples where high concentrations of background impurities and organic compounds are present. The straightforward procedures minimize error-introducing steps, require less time and materials, and result in an accurate method suitable for routine analyses.


1976 ◽  
Vol 65 (5) ◽  
pp. 738-740 ◽  
Author(s):  
R.J. Warren ◽  
J.E. Zarembo ◽  
D.B. Staiger ◽  
A. Post

2012 ◽  
Vol 61 (11) ◽  
pp. 963-967 ◽  
Author(s):  
Taichi YAMAZAKI ◽  
Takeshi SAITO ◽  
Tooru MIURA ◽  
Toshihide IHARA

1978 ◽  
Vol 56 (6) ◽  
pp. 789-793 ◽  
Author(s):  
Donald C. Wigfield ◽  
Steve Feiner

The stereoisomers of 2-methyltetrahydropyran-4-ol have been separated and identified by carbon-13 and proton nmr analysis of the trideuteriomethyl-2,6,6-trideuterio analogue. Stereoisomeric product ratios of reduction of 2-methyltetrahydropyran-4-one (1) by NaBH4, KBH4, L-Selectride, K-Selectride, and LiBH(nBu)3 have been determined and compared with reductions of 3-methylcyclohexanone. Product ratios in the reduction of the two substrates by the borohydride reducing agents are similar but are quite different in the reduction by the Selectride reducing agents, 1 being reduced by Selectride to give 73% equatorialalcohol. Two possible mechanisms of reduction of 1 are proposed, involving intramolecular assistance by the cyclic ether oxygen.


1974 ◽  
Vol 6 (8) ◽  
pp. 452-453 ◽  
Author(s):  
A. F. Cockerill ◽  
R. C. Harden ◽  
G. L. O. Davies ◽  
D. M. Rackham

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