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CAS No. : | 473596-87-1 | MDL No. : | MFCD08669595 |
Formula : | C15H21BO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | RDBWYSWPXDSHOE-UHFFFAOYSA-N |
M.W : | 276.14 | Pubchem ID : | 11087024 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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* 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 |
---|---|---|
With sodium carbonate;dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2; In ethanol; at 80℃; for 3h;Product distribution / selectivity; | <strong>[452-92-6]5-bromo-2,4-difluoroaniline</strong> (500 mg, 2.40 mmol), methyl 3-methyl-4-(4,4,5,5-tetramethyl-l,3,2- dioxaborolan-2-yl)benzoate (BSfTERMEDIATE 16, 797 mg, 2.88 mmol), sodium carbonate (2.40 mL, aq., 2M, 2.88 mrnol), l,l'-bis(diphenylphosphino) ferrocene-palladium dichloride dichloromethane adduct (196 mg, 0.24 mmol) and ethanol (15 ml) were heated in an 80 0C oil bath for 3 hours then allowed to cool to ambient overnight. Volatiles were removed under reduced pressure. The pot residue was worked up w/DCM /brine/Na2Sthetayfltratio:n/concentration to afford a dark oil. The resulting oil was purified by flash chromatography (SiO2, Biotage 40+M cartridge). The column was eluted by a 0% to 40% EtOAc/hexa?es gradient mixture. Related fractions were pooled and concentrated in vacuo to afford the title compound. LCMS (ESI) calc. = 277.09; found = 278.03 (M+l)+.; Step A methyl 5'-amino-2',4'-difluoro-2-methylbiphenyl-4-carboxyIate<strong>[452-92-6]5-bromo-2,4-difluoroaniline</strong> (500 mg, 2.40 mmol), methyl 3-methyl-4-(4,4,5,5-tetrarnethyl-l,3,2- dioxaborolan-2-yl)benzoate (INTERMEDIATE 16, 797 mg, 2.88 mmol), sodium carbonate (2.40 mL, aq., 2M, 2.88 mmol), l,r-bis(diphenylphosphino) ferrocene-palladium dichloride dichloromethane adduct (196 mg, 0.24 mmol) and ethanol (15 ml) were heated in an 80 0C oil bath for 3 hours then <n="146"/>allowed to cool to ambient overnight. Volatiles were removed under reduced pressure. The pot residue was worked up w/DCM /brine/Na2SCVfltration/concentration to afford a dark oil. The resulting oil was purified by flash chromatography (SiO2, Biotage 40+M cartridge). The column was eluted by a 0% to 40% EtOAc/hexanes gradient mixture. Related fractions were pooled and concentrated in vacuo to afford the title compound. LCMS (ESI) calc. = 277.09; found = 278.03 (M+l)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70 mg | With potassium fluoride; tetrakis(triphenylphosphine) palladium(0); tri tert-butylphosphoniumtetrafluoroborate; In tetrahydrofuran; water; at 20℃; for 14h;Inert atmosphere; | Preparation Example 5 Under an argon gas atmosphere, tris(dibenzylideneacetone)dipalladium (14 mg) and tri-tert-butylphosphonium tetrafuloroborate (11 mg) were added to a mixture of <strong>[425379-16-4]2-bromo-3-fluorobenzonitrile</strong> (150 mg), 4-methoxycarbonyl-2-methylphenylboronic acid pinacol ester (259 mg), potassium fluoride (144 mg), THF (1.8 mL), and water (0.23 mL), followed by stirring for 14 hours at room temperature. The reaction liquid was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate), thereby obtaining methyl 2'-cyano-6'-fluoro-2-methylbiphenyl-4-carboxylate (70 mg). |