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Deem, Madeleine C. ; Hein, Jason E. ; JOC,2023,88(2):1292-1297. DOI: 10.1021/acs.joc.2c02737 PubMed ID: 36625157
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Abstract: Online HPLC reaction progress monitoring provides detailed data-rich profiles; however, extracting kinetic information requires UV-visible response factors to determine concentrations from peak areas. If the reaction's overall mass balance is known and some anal. trend for all relevant species can be recorded, it is possible to estimate the absolute response factors of all species using a system of linear equations. We delineate a method using the Microsoft Solver plug-in to convert time course profiles to reagent concentrations without anal. standards
Purchased from AmBeed: 207739-72-8 ; 128055-74-3 ; 101-70-2 ; 28320-32-3 ; 501-65-5 ; 103-30-0 ; 1754-62-7 ; 17619-97-5
CAS No. : | 128055-74-3 | MDL No. : | MFCD08704220 |
Formula : | C25H12Br4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MASXXNUEJVMYML-UHFFFAOYSA-N |
M.W : | 631.98 | Pubchem ID : | 371282 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H319 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate In toluene at 110℃; for 12 h; Inert atmosphere | Nitrogen gas in 50 mL 2-necked flask, the 4,4'-dimethoxydiphenylamine (2.00 g, 8.72 mmol), 2,2',7,7'-tetrabromo-9,9'-spirobi[9H-fluorene] (1.23 g, 1.94 mmol), sodium tertbutoxide (1.12 g, 11.6 mmol), tris (dibenzylideneacetone) dipalladium (0) (0.071 g, 0.078 mmol) and tri-tert-butylphosphine (0.025 g, 0.12 mmol) to put this in dry toluene 15mL was added to 110 °C and stirred for 12 hours. The reaction mixture was cooled to room temperature and extracted with ethyl acetate and dried with washed with brine MgSO4 The solvent was removed by separation and purification by column chromatography (ethyl acetate / hexane = 1/2) of the solid of the title compound as a beige It was obtained (45percent, 1.07 g) |