To determine yield by NMR You will be determining the yield of your reaction through the use of an internal standard. This works by calculating the relative ratio of your product (P), to a known amount of added internal standard (IS). This is a common method for assaying reactions when developing new methodologies. The ratio of compounds in a sample can be determined by using the integrals of the corresponding peaks. This ratio needs to be corrected for the number of nuclei represented by the peaks chosen in order to give the molar ratio of the compounds. YOUR TA WILL TAKE NMR FOR YOU AND PROVIDE YOU WIH NESSISARY DATA. To calculate the ratio, you will need the integrals of peaks for the product (P) and the internal standard HMDSO (IS), and the corresponding proton number (N) for the represented peaks. You will be integrating the methyl peak of the ketone (8=2.5 ppm, 3H), and the HMDSO peak (8 = 0.0 ppm, 18H). Τρ (integralp\ = (integ gralp)/(integralis) Np The equation can be simplified by substituting in the N values, which gives: (integralp)/ (integra Τρ ris 3 18 To determine the molar amount of product, the ratio is multiplied by the molar amount of internal standard that was added to the solution. (nis = 0.047 mmol). rp np = nis ; np = 0.047 mmol тр TIS TIS Use the molar amount of product to calculate yield by dividing by the theoretical molar amount of product. np * 100 % Yield = (theo.)
To determine yield by NMR You will be determining the yield of your reaction through the use of an internal standard. This works by calculating the relative ratio of your product (P), to a known amount of added internal standard (IS). This is a common method for assaying reactions when developing new methodologies. The ratio of compounds in a sample can be determined by using the integrals of the corresponding peaks. This ratio needs to be corrected for the number of nuclei represented by the peaks chosen in order to give the molar ratio of the compounds. YOUR TA WILL TAKE NMR FOR YOU AND PROVIDE YOU WIH NESSISARY DATA. To calculate the ratio, you will need the integrals of peaks for the product (P) and the internal standard HMDSO (IS), and the corresponding proton number (N) for the represented peaks. You will be integrating the methyl peak of the ketone (8=2.5 ppm, 3H), and the HMDSO peak (8 = 0.0 ppm, 18H). Τρ (integralp\ = (integ gralp)/(integralis) Np The equation can be simplified by substituting in the N values, which gives: (integralp)/ (integra Τρ ris 3 18 To determine the molar amount of product, the ratio is multiplied by the molar amount of internal standard that was added to the solution. (nis = 0.047 mmol). rp np = nis ; np = 0.047 mmol тр TIS TIS Use the molar amount of product to calculate yield by dividing by the theoretical molar amount of product. np * 100 % Yield = (theo.)
Chapter4: Least-squares And Calibration Methods
Section: Chapter Questions
Problem 1P
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Transcribed Image Text:To determine yield by NMR
You will be determining the yield of your reaction through the use of an internal standard. This works by
calculating the relative ratio of your product (P), to a known amount of added internal standard (IS). This
is a common method for assaying reactions when developing new methodologies. The ratio of compounds
in a sample can be determined by using the integrals of the corresponding peaks. This ratio needs to be
corrected for the number of nuclei represented by the peaks chosen in order to give the molar ratio of the
compounds. YOUR TA WILL TAKE NMR FOR YOU AND PROVIDE YOU WIH NESSISARY DATA.
To calculate the ratio, you will need the integrals of peaks for the product (P) and the internal standard
HMDSO (IS), and the corresponding proton number (N) for the represented peaks. You will be
integrating the methyl peak of the ketone
(8=2.5 ppm, 3H), and the HMDSO peak (8 = 0.0 ppm, 18H).
Τρ
(integralp\
= (integ gralp)/(integralis)
Np
The equation can be simplified by substituting in the N values, which gives:
(integralp)/ (integra
Τρ
ris
3
18
To determine the molar amount of product, the ratio is multiplied by the molar amount of internal
standard that was added to the solution. (nis = 0.047 mmol).
rp
np =
nis
; np = 0.047 mmol
тр
TIS
TIS
Use the molar amount of product to calculate yield by dividing by the theoretical molar amount of
product.
np
* 100
% Yield = (theo.)
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