chapter 2 palladium catalysts in suzuki cross- coupling reaction

pA
800
600
400
200
FID1 A, (ORTAK\ORTAK094\G180SUZ1.D)
4-bromoanisole
0
0 2 4 6 8 10 12 14 16 18
9.529
hexadecane
14.516
15.325
4-methoxybiphenyl
Figure 4.3. GC chromatogram of a selected Suzuki Reaction (4-bromoanisole and
phenylboronic acid)
4.3.1.1. Calculation of Reactant and Product Amount on GC
For the calculation of amount of reactants and products, response factor of each
reactant and product for the set temperature program of GC was determined. As internal
standard, hexadecane was used. The amount of internal standard does not change
throughout the reaction, so the response factor of each compound was determined
according to the amounts and areas under the peaks of internal standard and standard
compound of interest. For the determination of response factor of a compound, a known
amount of standard compound together with a known amount of internal standard
dissolved in the reaction solvent and diluted with ethyl acetate, and then was injected to
GC. After the analysis is complete according to the set temperature program, the
following equation is used for the determination of response factor of that compound:
R.F. =
internal standart area
compound area
compound amount
x (4.2)
internal standart amount
In Suzuki experiments response factor values for the reactant and products were
determined with respect to hexadecane as internal standard. In order to calculate the
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