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CAS No. : | 133997-05-4 | MDL No. : | MFCD04039034 |
Formula : | C14H23BO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HUKDAABRKOWPNA-UHFFFAOYSA-N |
M.W : | 234.14 | Pubchem ID : | 4197992 |
Synonyms : |
|
Chemical Name : | (4-Octylphenyl)boronic acid |
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: |
* 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 |
---|---|---|
Under nitrogen atmosphere, 10 ml of a solution of 1.6M n-butyl lithium (16 mmol) in hexane is put into a 100 ml three-necked flask cooled at -80 C. After cooling to -80 C., 10 ml of THF is added dropwise thereto using a dropping funnel while the THF is maintained at -60 C. Thereafter, 3.1 g (16 mmol) of 1-bromo-4-n-octylbenzene maintained at -60 C. is added dropwise thereto using a dropping funnel. The resultant mixture is stirred at -40 C. for 1 hour, and a solution of 2.3 g (22 mmol) of trimethyl borate in 10 ml of THF is added dropwise to the mixture using a dropping funnel while the temperature of the added solution is maintained at -40 C. Thereafter, the temperature of the mixture is gradually increased to 10 C. over 2 hours, and 50 ml of a 10% HCl aqueous solution is added thereto at 0 C., and extraction is performed using 100 ml of toluene. The extract is washed with 100 ml of pure water three times, and is dehydrated using sodium sulfate. Toluene is distilled off by reducing the pressure, whereby remaining matter in an amount of 3.3 g is obtained. The remaining matter is washed with a mixed solution of 100 ml pure water/100 ml hexane, whereby 2.0 g of Compound V-a, which is 4-n-octylphenyl borate, is obtained. The obtained compound is identified as the desired product by 1H-NMR and IR. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In 1,2-dimethoxyethane; water;Heating / reflux; | Part B: Preparation of 4'-nitro-4-n-octyl-biphenyl <n="43"/>[0115] Tetrakis(triphenylphosphine)palladium (0) (0.30 g, 0.26 mmol) and p-n- octylphenylboronic acid (1.0 g, 4.3 mmol) were sequentially added to a stirred solution of 4-nitroiodobenzene (0.87 g, 3.5 mmol) in 1 ,2-dimethoxyethane (13 mL) and aqueous sodium carbonate (2 M, 13 mL) under dry nitrogen. The stirred mixture was heated under reflux overnight and cooled. Water was added and the product was extracted into ether (30><3 mL) and the combined ethereal extracts were washed with brine and dried with MgSO4. The solvent was removed in vacuo and the residue was purified by chromatography using a short silica gel column (hexane:ethyl acetate - 5: 1 to 2:1] to provide 4'-nitro-4-n-octyl-biphenyl as a yellow oil, which solidified upon standing (1.04 g, 95% yield). The solid was used without further purification.[0116] 1H NMR (CDCl3) delta 0.90 (3H, t), 1.19-1.58 (1OH, m), 1.67 (2H, quint), 2.68 (2 H, t), 7.31(2H, d, J=8.5 Hz), 7.56(2H, d, J=8.5 Hz), 7.73 (2H, d, J=9.0 Hz), 8.29 (2H, d, J=9.0 Hz); GC MS w/z=311 (M+). |
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